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BRITISH STANDARD BS EN 196-6:2010

Methods of testing
Licensed copy: Bradford University, University of Bradford, Version correct as of 05/02/2012 14:46, (c) The British Standards Institution 2012

cement
Part 6: Determination of fineness

ICS 91.100.10

NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW


BS EN 196-6:2010

National foreword
Licensed copy: Bradford University, University of Bradford, Version correct as of 05/02/2012 14:46, (c) The British Standards Institution 2012

This British Standard is the UK implementation of EN 196-6:2010. It


supersedes BS EN 196-6:1992 which is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee B/516, Cement and lime.
A list of organizations represented on this committee can be obtained on
request to its secretary.
The European Standard specifies the use of a 'reference material of
known sieve residue' for checking the sieve in the sieving method
(clause 3). National Annex NA gives a suitable reference material for
the UK.
The European Standard furthermore specifies the use of a 'reference
cement of known specific surface' for the determination of the
'apparatus constant' in the air permeability method (Blaine method)
(clause 4). National Annex NB describes a procedure previously given in
BS 4550 for measuring the 'absolute' specific surface of a possible,
future reference cement, ideally sourced within Europe, for use with
this European Standard.
The European Standard includes in 4.5.3 only the principle of the
method of determination of density which is required for the air
permeability methods. National Annex NC therefore describes in full a
procedure for determining the density of cement.
National Annex ND indicates UK preferred methods for the reporting of
the results.
National Annex NE gives details of corresponding British Standards for
International Standards referred to in the European Standard.
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 Amendments/corrigenda issued since publication


was published under the
authority of the Standards
Policy and Strategy Date Comments
Committee on 30 April
2010.
© BSI 2010

ISBN 978 0 580 62238 0


BS EN 196-6:2010

EUROPEAN STANDARD EN 196-6


NORME EUROPÉENNE
EUROPÄISCHE NORM January 2010
Licensed copy: Bradford University, University of Bradford, Version correct as of 05/02/2012 14:46, (c) The British Standards Institution 2012

ICS 91.100.10 Supersedes EN 196-6:1989

English Version

Methods of testing cement - Part 6: Determination of fineness

Méthodes d'essai des ciments - Partie 6: Détermination de Prüfverfahren für Zement - Teil 6: Bestimmung der
la finesse Mahlfeinheit

This European Standard was approved by CEN on 21 December 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.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, 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

© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 196-6:2010: E
worldwide for CEN national Members.
BS EN 196-6:2010
EN 196-6:2010 (E)
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Contents Page

Foreword ..............................................................................................................................................................3
1 Scope ......................................................................................................................................................5
2 Normative references ............................................................................................................................5
3 Sieving method ......................................................................................................................................5
3.1 Principle ..................................................................................................................................................5
3.2 Apparatus ...............................................................................................................................................5
3.3 Material for checking the sieve ............................................................................................................6
3.4 Procedure ...............................................................................................................................................6
3.5 Expression of results ............................................................................................................................7
4 Air permeability method (Blaine method) ...........................................................................................7
4.1 Principle ..................................................................................................................................................7
4.2 Apparatus ...............................................................................................................................................7
4.3 Materials .............................................................................................................................................. 10
4.4 Test conditions ................................................................................................................................... 10
4.5 Compacted cement bed ..................................................................................................................... 10
4.6 Air permeability test ........................................................................................................................... 11
4.7 Calibration of apparatus .................................................................................................................... 12
4.8 Special cements .................................................................................................................................. 14
4.9 Simplification of the calculations...................................................................................................... 15
4.10 Expression of results ......................................................................................................................... 16
5 Air-jet sieving method ........................................................................................................................ 16
5.1 Principle ............................................................................................................................................... 16
5.2 Apparatus ............................................................................................................................................ 17
5.3 Procedure ............................................................................................................................................ 18
5.4 Checking the sieve ............................................................................................................................. 18
5.5 Expression of results ......................................................................................................................... 18
5.6 Repeatability and reproducibility ...................................................................................................... 18

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BS EN 196-6:2010
EN 196-6:2010 (E)
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Foreword
This document (EN 196-6:2010) has been prepared by Technical Committee CEN/TC 51 “Cement and
building limes”, the secretariat of which is held by NBN.

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 July 2010, and conflicting national standards shall be withdrawn at the
latest by July 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 196-6:1989.

EN 196, 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 times and soundness

 Part 5: Pozzolanicity test for pozzolanic cement

 Part 6: Determination of fineness

 Part 7: Methods of taking and preparing samples of cement

 Part 8: Heat of hydration — Solution method

 Part 9: Heat of hydration — Semi-adiabatic method

 Part 10: Determination of the water-soluble chromium (VI) content of cement

NOTE A previous part, EN 196-21, Methods of testing cement — Determination of the chloride, carbon dioxide and
alkali content of cement, has been revised and incorporated into EN 196-2.

Another document, ENV 196-4, Methods of testing cement — Quantitative determination of constituents, has
been published as CEN/TR 196-4, Methods of testing cement — Part 4: Quantitative determination of
constituents.

This edition introduces the following technical changes based on comments received by the Secretariat:

a) A method to determine the residue on sieving by air-jet equipment is included;

b) The method for calibration of the air permeability equipment has been clarified and an alternative method,
avoiding the use of mercury, added;

c) The factors used in the air permeability (Blaine) method have been corrected for errors introduced in the
conversion to SI units.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech

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BS EN 196-6:2010
EN 196-6:2010 (E)

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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BS EN 196-6:2010
EN 196-6:2010 (E)

1 Scope
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This European Standard describes three methods of determining the fineness of cement.

The sieving method serves only to demonstrate the presence of coarse cement particles. This method is
primarily suited to checking and controlling the production process.

The air-jet sieving method measures the retention on sieving and is suitable for particles which substantially
pass a 2,0 mm test sieve. It may be used to determine the particle size distribution of agglomerates of very
fine particles. This method may be used with test sieves in a range of aperture sizes, e.g. 63 µm and 90 µm.

The air permeability method (Blaine) measures the specific surface (mass related surface) by comparison with
a reference cement sample. The determination of the specific surface serves primarily to check the
consistency of the grinding process of one and the same plant. This method only enables a limited
assessment to be made of the properties of the cement in use.

NOTE The air permeability method may not give significant results for cements containing ultrafine materials.

The methods are applicable to all the cements defined in EN 197.

2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.

EN 197-1, Cement ― Part 1: Composition, specifications and conformity criteria for common cements

ISO 383:1976, Laboratory glassware ― Interchangeable conical ground joints

ISO 565, Test sieves ― Metal wire cloth, perforated metal plate and electroformed sheet ― Nominal sizes of
openings

ISO 3310-1, Test sieves ― Technical requirements and testing ― Part 1: Test sieves of metal wire cloth

ISO 4803, Laboratory glassware ― Borosilicate glass tubing

3 Sieving method

3.1 Principle

The fineness of cement is measured by sieving it on standard sieves. The proportion of cement of which the
grain sizes are larger than the specified mesh size is thus determined.

A reference sample having a known proportion of material coarser than the specified mesh size is used for
checking the specified sieve.

3.2 Apparatus

3.2.1 Test sieve, comprising a firm, durable, non-corrodible, cylindrical frame of 150 mm to 200 mm
nominal diameter and 40 mm to 100 mm depth, fitted with, e.g. 90 µm, mesh sieve cloth of woven stainless
steel, or other abrasion-resisting and non-corrodible metal wire.

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BS EN 196-6:2010
EN 196-6:2010 (E)

The sieve cloth shall conform to the requirements of ISO 565 and ISO 3310-1 and shall be free of visible
irregularities in mesh size when inspected optically by the methods of ISO 3310-1. A tray fitting beneath the
sieve frame and a lid fitting above it shall be provided to avoid loss of material during sieving.
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NOTE Sieving may be carried out manually or on a sieving machine.

3.2.2 Balance, capable of weighing up to 25 g to the nearest 0,01 g.

3.3 Material for checking the sieve

A reference material of known sieve residue shall be provided for checking the sieve.

The material shall be stored in sealed, airtight containers to avoid changes in its characteristics due to
absorption or deposition from the atmosphere. The containers shall be marked with the sieve residue of the
reference material.

3.4 Procedure

3.4.1 Determination of the cement residue

Agitate the sample of cement to be tested by shaking for 2 min in a stoppered jar to disperse agglomerates.
Wait 2 min. Stir the resulting powder gently using a clean dry rod to distribute the fines throughout the cement.

Fit the tray under the sieve. Weigh (25 ± 0,5) g of cement to the nearest 0,01 g and place it in the sieve, being
careful to avoid loss. Disperse any agglomerates. Fit the lid over the sieve. Agitate the sieve by swirling,
planetary and linear movements until no more fine material passes through it.

Remove and weigh the residue. Express its mass as a percentage, R1 of the quantity first placed in the sieve
to the nearest 0,1 %. Gently brush all the fine material off the base of the sieve into the tray.

Repeat the whole procedure using a fresh 25 g sample to obtain R2. Then calculate the residue of the cement
R as the mean of R1 and R2 as a percentage, expressed to the nearest 0,1 %.

When the results differ by more than 1 % absolute, repeat the whole procedure a third time and calculate the
mean of the three values.

Sieving by the manual process requires a skilled and experienced operator.

3.4.2 Checking the sieve

Sieves should be cleaned and checked for damage after each sieving (e.g. that the mesh is taut and is not
dented or perforated). In addition, check the sieve after every 100 sievings as follows:

Agitate the sample of reference material, to be used for checking the sieve, by shaking for 2 min in a
stoppered jar to disperse agglomerates. Wait 2 min. Stir the resulting powder gently using a clean dry rod to
distribute the fines throughout the reference material.

Fit the tray under the sieve. Weigh (25 ± 0,5) g of the reference material (3.3) to the nearest 0,01 g and place
it in the sieve, being careful to avoid loss. Sieve the material in accordance with 3.4.1 including the repeat
determination of residue to yield two values P1 and P2 expressed to the nearest 0,1 %.

The two values of P1 and P2 for a satisfactory sieve should differ by not more than 0,6 %. Their mean P
characterizes the state of the sieve.

Given the known residue on the sieve of the reference material, R0, calculate R0IP as the sieve factor, F,
expressed to the nearest 0,01. The residue, R, determined as in 3.4.1 shall be corrected by multiplying by F,
which may have a value of 1,00 ± 0,20.

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BS EN 196-6:2010
EN 196-6:2010 (E)

When the factor F exceeds the permitted value, 1,00 ± 0,20, the sieve shall be discarded.

NOTE Any other checking procedure, such as the optical methods described in ISO 3310-1 may be used. All sieves
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will wear slowly and consequently their sieve factor, F, will slowly change.

3.5 Expression of results

Report the value of R to the nearest 0,1 %, as the residue, the sieve mesh size and details of the cement
tested.

The standard deviation of the repeatability is about 0,2 % and of the reproducibility is about 0,3 %.

NOTE Where there is local difficulty in obtaining ISO standard sieves, the same procedure can be followed with the
nearest available standard sieve but the report should state on which standard sieve mesh the cement residue has been
determined.

4 Air permeability method (Blaine method)

4.1 Principle

The fineness of cement is measured as specific surface by observing the time taken for a fixed quantity of air
to flow through a compacted cement bed of specified dimensions and porosity. Under standardized conditions
the specific surface of cement is proportional to √t where t is the time for a given quantity of air to flow through
the compacted cement bed. The number and size range of individual pores in the specified bed are
determined by the cement particle size distribution, which also determines the time for the specified air flow.

The method is comparative rather than absolute and therefore a reference sample of known specific surface is
required for calibration of the apparatus.

4.2 Apparatus

4.2.1 Permeability cell. The cell shall be a rigid right cylinder of the dimensions and tolerances shown in
Figure 1 a). It shall be of austenitic stainless steel or other abrasion-resisting, non-corrodible material. The top
and bottom faces shall be flat and normal to the axis of the cylinder, as shall the upper surface of the ledge at
the bottom of the cell. The outer surface of the cylinder shall be tapered to form an airtight fit with the conical
socket of the manometer (ISO 383:1976, Joint 19/34).

4.2.2 Perforated disc. The disc shall be of non-corrodible metal, perforated with 30 to 40 holes of
1 mm diameter, and shall have the dimensions and tolerances shown in Figure 1 b). When in position on the
ledge in the cell, its plane surfaces shall be normal to the axis of the cell.

4.2.3 Plunger. The plunger is a piston, capable of sliding freely in the measuring cell by means of a
clearance to be applied in such a way that, when the cap of the plunger comes to rest on the upper face of the
cell cylinder, a distance of (15 ± 1) mm will be maintained between the upper face of the perforated disc and
the lower face of the piston.

This piston shall be provided with a flat connected to an annulus around the head to enable air to escape.

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BS EN 196-6:2010
EN 196-6:2010 (E)

Dimensions in millimetres
G
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J
4

H
5

L
6 K

a) Cell b) Perforated disc

20* A

12
16*
13
7
13*
F = J-H

8
1

110

B
9
2

70
15

C
10
E
11
14
3*

15
2

* Recommended D

c) Plunger d) Manometer

Item Description
1 Piston
2 Flat for air vent
3 Cell
4 Compacted cement disc
5 Filter paper disc
6 Perforated disc
7 Manometer
8, 9, 10, 11 Etched lines
12 Conical joint for cell
13 Stopcock
14 Rubber tube
15 Aspirator bulb

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BS EN 196-6:2010
EN 196-6:2010 (E)

Key Recommended Key Obligatory


mm mm
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A Minimum dimension ≤ 50 G Cell diameter at 12,7 ± 0,1


between conical joint base of cell
and stopcock

B Dimension between 135 ± 10 E Diameter of G - 0,1


upper arm of T-joint plunger/piston
and lowest etched
line on arm of
manometer tube
C Dimension between 275 ± 25 H Height of cement 15 ± 1
upper arm of T-joint bed
and base of U-tube

D Dimension between 23 ± 1 F Dimension/depth J-H


centre lines of arms between tip of
of U-tube plunger and
shoulder
J Inner 50 ± 15
dimension/height of
the cell

K Width of cell ledge 0,8 ± 0,2

L Thickness of 0,9 ± 0,1


perforated disc

M Diameter of arms of 9,0 ± 0,4


manometer tube

Figure 1 — Blaine permeability apparatus

The plunger shall be of austenitic stainless steel or other abrasion-resisting and non-corrodible material; it
shall have the dimensions and tolerances shown in Figure 1 c). A plunger shall only be used with a cell of the
specified dimensions and tolerances such that, when used together, the specified distance between the upper
face of the perforated disc and the lower face of the piston is satisfied.

4.2.4 Manometer. The manometer shall be a rigidly and vertically mounted U-tube of borosilicate glass
tubing conforming to ISO 4803 arranged as in Figure 1 d) and having the dimensions and tolerances shown in
that figure.

One arm of the manometer shall be provided at the top with a conical socket conforming to ISO 383:1976,
Joint 19/34 to form an airtight fit with the conical surface of the cell. The same arm shall also have four etched
lines and a T-joint whose positions shall have the dimensions and tolerances shown in Figure 1 d). The side
branch of the T-joint shall lead to an airtight stopcock beyond which shall be attached a suitable aspiration
device such as the rubber tube and bulb shown in Figure 1 d).

Fill the manometer tube with the liquid (4.2.5) to wet the inner surface. Empty the tube and refill it so that the
manometer liquid is level with the lowest etched line (11 in Figure 1 d)). This manometer liquid shall be
changed (or cleaned) after servicing or before a new calibration.

NOTE Other forms of cell and plunger and other arrangements of the joint between cell and manometer may be used
provided that they can be shown to give the same results as the specified apparatus.

4.2.5 Manometer liquid. The manometer shall be filled to the level of the lowest etched line (11 in
Figure 1 d)) with a non-volatile, non-hygroscopic liquid of low viscosity and density, such as dibutyl phthalate
or light mineral oil.

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BS EN 196-6:2010
EN 196-6:2010 (E)

4.2.6 Timer, having a positive starting and stopping mechanism, readable to 0,2 s or better, and accurate
to 1 % or better over time intervals up to 300 s.
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4.2.7 Balance(s), capable of weighing about 3 g to the nearest 0,001 g (for the cement) and about 50 g to
110 g to the nearest 0,01 g (for the mercury).

4.2.8 Apparatus, to determine the density of cement, e.g. pyknometer or Le Chatelier flask.

4.3 Materials

4.3.1 Mercury, of reagent grade or better.

4.3.2 Reference cement, of known specific surface.

NOTE Results may vary when using cements of different types or when using cements of the same type from different
suppliers.

4.3.3 Light oil, to prevent formation of mercury amalgam on the inner surface of the cell.

4.3.4 Circular discs of filter paper, of medium porosity having a smooth circumference adapted to the
dimensions of the cell.

4.3.5 Light grease, for ensuring an airtight joint between cell and manometer, and in the stopcock.

4.4 Test conditions

The laboratory in which the air permeability test is carried out shall be maintained at a temperature of
(20 ± 2) °C and a relative humidity not exceeding 65 %. All materials for test and calibration shall be at the
laboratory temperature when used and shall be protected from absorption of atmospheric moisture during
storage.

4.5 Compacted cement bed

4.5.1 Basis

The compacted cement bed comprises a reproducible arrangement of cement particles with a specified
volume (see 4.5.4) of air included between the particles. This air volume is defined as a fraction of the total
volume of the bed and is termed the porosity, e.

It follows that the volume fraction occupied by the cement particles is (1 - e). If V is the total volume of the bed,
3
the absolute volume of cement is V(1 - e) in cubic centimetres (cm ), and the mass of cement, m is
p × V(1 − e) in grams (g) where p is the solid density of the cement particles in grams per cubic centimetre
3
(g/cm ).

Thus, knowing p, a mass of cement can be weighed to produce a desired porosity, e, in the compacted bed of
total volume V. The determination of p is described in 4.5.3 and that of V in 4.7.1.

4.5.2 Preparation of the sample

Agitate the sample of cement to be tested by shaking for 2 min in a stoppered jar to disperse agglomerates.
Wait 2 min. Stir the resulting powder gently using a clean dry rod to distribute the fines throughout the cement.

4.5.3 Determination of density

Determine the density of the cement using a device such as a pyknometer (4.2.8). Use a non-reactive liquid in
the determination. The quantity of cement used will depend on the nature of the apparatus but shall be such

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BS EN 196-6:2010
EN 196-6:2010 (E)

3
that the value of p determined is accurate to 0,01 g/cm . Verify this accuracy by a repeat determination and
3
record the mean of the two determinations to the nearest 0,01 g/cm as the density.
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4.5.4 Formation of the bed

To give a cement bed of porosity e = 0,500 weigh a quantity of cement, m1, calculated from

m1 = 0,500 ρV , in grams (g) (1)

where
3
ρ is the density of the cement in grams per cubic centimetre (g/cm ) (4.5.3);
3
V is the volume of the cement bed in cubic centimetres (cm ) (4.7.1).

This mass, correctly compacted, will produce a bed of porosity 0,500. Place the perforated disc (4.2.2) on the
ledge at the bottom of the cell (4.2.1) and place on it a new filter paper disc (4.3.4). Ensure that the filter paper
disc fully covers the perforated disc and is flat by pressing with a clean dry rod. Place the weighed quantity of
cement, m1, in the cell taking care to avoid loss. Tap the cell to level the cement. Place a second new filter
paper disc on the levelled cement. Insert the plunger (4.2.3) to make contact with the filter paper disc. Press
the plunger gently but firmly until the lower face of the cap is in contact with the cell. Slowly withdraw the
plunger about 5 mm, rotate it through 90° and gently but firmly press the bed once again until the plunger cap
is in contact with the cell. The bed is now compacted and ready for the permeability test. Slowly withdraw the
plunger.

NOTE Too rapid and vigorous pressing may change the particle size distribution and therefore change the specific
surface of the bed. The maximum pressure should be that comfortably exerted by a thumb on the plunger.

4.6 Air permeability test

4.6.1 Basis

The specific surface, S, is given in 4.9.1 but is conveniently expressed, in square centimetres per gram
(cm²/g), as

K e3 t
S= × × (2)
ρ (1 − e) 10 ×η

where

K is the apparatus constant (4.7.2);

e is the porosity of the bed;

t is the measured time in seconds (s);


3
ρ is the density of cement in grams per cubic centimetre (g/cm ) (4.5.3);

η is the viscosity of air at the test temperature taken from Table 1, in Pascal seconds (Pa·s).

With the specified porosity of e = 0,500 and temperature of (20 ± 2) °C:

S=
52,43 K × t
ρ
(cm / g )
2
(3)

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EN 196-6:2010 (E)

4.6.2 Procedure

Insert the conical surface of the cell into the socket at the top of the manometer, using if necessary a little light
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grease (4.3.5) to ensure an airtight joint. Take care not to disturb the cement bed.

Close the top of the cylinder with a plug. Open the stopcock and with gentle aspiration raise the level of the
manometer liquid to that of the highest etched line (8 in Figure 1 d)). Close the stopcock and observe that the
level of the manometer liquid remains constant. If it falls, remake the cell/manometer joint and check the
stopcock. Repeat the leakage test until the improved sealing produces a steady level of the liquid. Open the
stopcock and by gentle aspiration adjust the level of the liquid, to that of the highest etched line.

Close the stopcock. Remove the plug from the top of the cylinder. The manometer liquid will begin to flow.
Start the timer as the liquid reaches the second etched line (9 in Figure 1 d)) and stop it when the liquid
reaches the third etched line (10 in Figure 1 d)). Record the time, t, to the nearest 0,2 s and the temperature to
the nearest 1 °C.

Repeat the procedure on the same bed and record the additional values of time and temperature. Prepare a
fresh bed of the same cement with a second sample following the procedure of 4.5.4 or, where there is little
cement available, by breaking up the first bed and reforming it as in 4.5.4. Carry out the permeability test twice
on the second bed, recording the values of time and temperature as before.

4.7 Calibration of apparatus

4.7.1 Determination of the bed volume

NOTE In some countries there are restrictions on the use of mercury in the laboratory. To overcome such restrictions
the alternative determination set out in 4.7.1.2 may be used. A limited number of comparative tests has indicated a
standard deviation of repeatability between the methods of less than 0,5 %.

4.7.1.1 Determination by mercury volume

Owing to the need for clearance between the cell and the plunger, the volume of the compacted cement bed
varies for each cell-plunger combination. The volume of the compacted cement bed shall be established for a
given cell-plunger clearance. This volume is to be determined as follows.

Apply a very thin film of light mineral oil (4.3.3) to the cell interior. Place the perforated disc on the ledge in the
cell. Place two new filter paper discs on the perforated disc and ensure that each covers the base of the cell
whilst lying flat by pressing with a rod.

Fill the cell with mercury (4.3.1). Remove any air bubbles with a clean dry rod. Ensure that the cell is full by
pressing a glass plate on the mercury surface until it is flush with the cell top. Empty the cell, weigh the
mercury to the nearest 0,01 g, m2, and record the temperature. Remove one filter paper disc. Using a trial
quantity of 2,90 g of cement (see Note 1) form a compacted cement bed (see Note 2) using the method
described in 4.5.4 and place on it a new filter paper disc. Refill the cell with mercury, removing air bubbles and
levelling the top as before. Remove the mercury, weigh it to the nearest 0,01 g, m3, and check the
temperature.

The bed volume V is given by

V =
m2 − m3
ρ Hg
(cm )
3
(4)

where

ρHg is the density of mercury at the test temperature taken from Table 1.

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BS EN 196-6:2010
EN 196-6:2010 (E)

Repeat the procedure with fresh cement beds until two values of V are obtained differing by less than
3
0,005 cm . Record the mean of these two values as V.
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WARNING — Care should be taken to avoid spilling or splashing the mercury and any contact
between it and the operator's skin and eyes.

NOTE 1 It is not necessary either to use the reference cement (4.3.2) or to achieve a particular bed porosity in the
determination of the bed volume.

NOTE 2 The compacted bed of cement should be firm. If it is too loose or if the cement cannot be compacted to the
point where the lower face of the cap is in contact with the cell (see 4.5.4), the trial quantity of cement should be adjusted.

4.7.1.2 Determination by measurement

4.7.1.2.1 Apparatus

4.7.1.2.1.1 Depth gauge, accurate to 0,01 mm

4.7.1.2.1.2 Internal micrometer, accurate to 0,01 mm

4.7.1.2.2 Procedure

Calibrate the cement bed volume by dimensional measurements in a room maintained at a temperature of
(20 ± 2) °C and with a relative humidity not exceeding 65 %.

Carry out all dimensional measurements to the nearest 0,01 mm.

Place two filter paper discs on the perforated disc placed at the bottom of the cell. Measure the inner
dimension (height: J) of the cell with a depth gauge. Repeat five times and record the mean to the nearest
0,01 mm.

Stand the plunger on its cap and, using the depth gauge, measure the length of the plunger inside the cell (F)
as the "depth" from the tip to the shoulder. Repeat five times and record the mean to the nearest 0,01 mm.

Measure the cell diameter (G) at the bottom (where the cement bed is formed) with the internal micrometer to
obtain its radius (r = G/2). Repeat five times and record the mean to the nearest 0,01 mm.

Calculate the cement bed height (H) to the nearest 0, 01 mm as J – F.


3
The bed volume (V), in cubic centimetres (cm ), is given by:
2
V = H × r × 3,14/1 000 (5)

where

H is the cement bed height, in millimetres (mm);

r is the radius of the cell, in millimetres (mm).


3 3
Record the result in cubic centimetres (cm ) to the nearest 0,001 cm .

4.7.2 Determination of the apparatus constant

From a supply of reference cement of known specific surface (4.3.2) prepare a compacted cement bed and
measure its permeability by the procedures given in 4.5.2, 4.5.3, 4.5.4 and 4.6.2. Record the time, t, and the
temperature of test. Using the same bed repeat twice the procedure of 4.6.2 and record the two further values

13
BS EN 196-6:2010
EN 196-6:2010 (E)

of time and of temperature. Repeat the whole on two further samples of the same reference cement. For each
of the three samples calculate the means of the three times and temperatures. For each sample calculate
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S 0 ρ 0 (1 − e) 10 ×η 0
K = (6)
e3 t0

where
2
S0 is the specific surface of the reference cement in square centimetres per gram (cm /g);
3
ρ0 is the density of the reference cement in grams per cubic centimetre (g/cm );

t0 is the mean of the three measured times in seconds (s);

η0 is the air viscosity at the mean of the three temperatures, in Pascal seconds (Pa·s) (Table 1).

With the specified porosity of e = 0,500,

10 × η 0
K = 1,414 S 0 ρ 0 (7)
t0

Take the mean of the three values of K as the constant K for the apparatus.

4.7.3 Recalibration

Repeated use of the apparatus may cause changes in the cement bed volume and in the apparatus constant
(because of the wear of cell, plunger and perforated disc). These changes can be determined with the help of
a so-called secondary reference cement whose specific surface has been measured. The cement bed volume
and the apparatus constant shall be recalibrated with the reference cement:

a) after 1 000 tests;

b) when another type of filter paper or a new perforated disc is used;

c) when systematic deviations of the secondary reference cement results are noted;

d) when another type of manometer fluid and/or a new manometer tube have been introduced the apparatus
constant only shall be recalibrated with the reference cement.

4.8 Special cements

Certain cements having unusual particle size distributions and, in particular, fine cements of higher strength
grades may prove difficult to form into a compacted bed of porosity e = 0,500 by the method of 4.5.4. Should
thumb pressure on the plunger cap fail to bring it in contact with the top of the cell or if, after making contact
and removing the pressure the plunger moves upwards, the porosity of e = 0,500 shall be considered
unattainable.

For such cases the porosity required for a well-compacted bed shall be determined experimentally. The mass
of cement, m4, weighed to make the bed as in 4.5.4 then becomes, in grams (g):

m4 = (1 − e1 ) ρ1 V (8)

where

e1 is the porosity determined experimentally.

14
BS EN 196-6:2010
EN 196-6:2010 (E)

4.9 Simplification of the calculations

4.9.1 Basic equation


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The specific surface, S, of the cement under test is calculated, in square centimetres per gram (cm²/g), from
Equation (9):

ρ 0 (1 − e0 ) e3 10 × η 0 t
S = × × × × × S0 (9)
ρ (1 − e) e0 3 10 × η t0

where
2
So is the specific surface of the reference cement in square centimetres per gram (cm /g) (4.3.2);

e is the porosity of the bed of cement under test;

eo is the porosity of the bed of reference cement (4.7.2);

t is the measured time for the cement under test in seconds (s);

to is the mean of the three times measured on the reference cement in seconds (s) (4.7.2);
3
ρ is the density of the cement under test in grams per cubic centimetre (g/cm ) (4.5.3);
3
ρ o is the density of the reference cement in grams per cubic centimetre (g/cm ) (4.7.2);

η is the air viscosity at the test temperature taken from Table 1, in Pascal seconds (Pa·s);

ηo is the air viscosity at the mean of the three temperatures (Table 1) for the reference cement, in
Pascal seconds (Pa·s).

4.9.2 Effect of specified porosity

Use of the specified porosity, e = 0,500, for both the reference and test cements simplifies Equation (9) to

ρ0 10× η 0 t 2
S = x × × S0 in square centimetres per gram (cm /g) (10)
ρ 10× η t0

In the case of cements requiring a porosity other than e = 0,500, Equation (10) cannot be used unless a
reference cement has been tested at that porosity.

4.9.3 Effect of controlled temperature

As will be seen in Table 1, the value of 10× η ranges from 0,013 454 at 18 °C to 0,013 524 at
22 °C. Under the specified laboratory conditions a value of 0,013 49 can be taken to apply with an extreme
error of 0,5 % and a more probable error of 0,3 % or less. This further simplification leads to the following
equation:

ρ0 t 2
S = × × S 0 in square centimetres per gram (cm /g) (11)
ρ t0

15
BS EN 196-6:2010
EN 196-6:2010 (E)

4.9.4 Effect of density of cement

The only remaining possibility of simplification is the elimination of the density (ρ) terms. This has previously
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been done where the only cements in question were pure Portland cements for which a value of ρ of 3,15 was
assumed to apply. That assumption is known to produce errors of up to 1 %. With the increasing use of
CEM II, III and IV cements (see EN 197-1) much greater errors are certain.

4.10 Expression of results

Where the porosity is e = 0,500, the four times and temperatures resulting from the procedure of 4.6.2 shall be
examined to check that the temperatures all fall within the specified range of (20 ± 2) °C. If they do, the mean
of the four times shall be inserted in Equation (3) or Equation (11) and the resulting value of S, to the nearest
2
10 cm /g, shall be reported as the specific surface of the cement.

A difference of 1 % between the means of the fineness measurements carried out on two different powder
beds from one and the same sample is acceptable.
2
The standard deviation of the repeatability is approximately 50 cm /g and of the reproducibility is
2
approximately 100 cm /g.
2
Where the porosity is not e = 0,500, Equation (9) shall be used and the result to the nearest 10 cm /g reported
as the specific surface of the cement.

If, owing to a breakdown in control or for other reasons, the four temperatures do not lie within the specified
range of (20 ± 2) °C, a value of S shall be calculated for each combination of time and temperature using
Equation (3) (where e = 0,500) or Equation (9) (where e ≠ 0,500). The mean of the four values of S shall be
2
reported, to the nearest 10 cm /g, as the specific surface of the cement.
2
NOTE To report the specific surface of the cement in SI units to the nearest m /kg, it is recommended to take the
resulting value of S and divide it by 10.

a
Table 1 — Density of mercury ρHg, viscosity of air η and 10×η as function of the temperatures
Temperature Density of mercury Viscosity of air η 10 × η
ρHg
3
°C g/cm Pa·s

16 13,560 0,000 018 00 0,013 416


17 13,560 0,000 018 05 0,013 435
18 13,550 0,000 018 10 0,013 454
19 13,550 0,000 018 15 0,013 472
20 13,550 0,000 018 19 0,013 487
21 13,540 0,000 018 24 0,013 506
22 13,540 0,000 018 29 0,013 524
23 13,540 0,000 018 34 0,013 543
24 13,540 0,000 018 39 0,013 561
a
Intermediate values shall be obtained by linear interpolation.

5 Air-jet sieving method

5.1 Principle

The method determines the retention on sieving of particles which substantially pass a 2,0 mm test sieve. The
method can be used to determine the particle size distribution of the agglomerates of very fine particles. This
method customarily uses test sieves with aperture sizes 63 µm or 90 µm.

16
BS EN 196-6:2010
EN 196-6:2010 (E)

NOTE Sieves with other aperture sizes may be used, preferably conforming to ISO 565.

5.2 Apparatus
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5.2.1 Air-jet sieving apparatus of the general form shown in Figure 2. The apparatus shall be set to give a
pressure difference of 2 kPa to 2,5 kPa across the sieve.

5.2.2 Test sieves, 200 mm diameter, aperture sizes e.g. 63 µm and 90 µm.

NOTE The effective operation of some makes of air-jet apparatus can necessitate non-standard sieve frames and
additional gaskets. In this case the sieving medium and general method of construction should comply with the
requirements of this standard.

5.2.3 Trays or other suitable containers of sufficient size to contain the test portion.

5.2.4 Balance, capable of weighing up to 25 g to the nearest 0,01 g.

5.2.5 Soft brush, for cleaning the mesh of the sieves, for example a camel hair brush.

5.2.6 Mallet, if there is a tendency for material to adhere to the lid of the apparatus. A rubber or plastic
tipped mallet is preferred.

5.2.7 Ventilated drying oven (optional), thermostatically controlled to maintain a temperature of


(105 ± 5) °C.

4 8 9 7

6 1
2
5 10
12
11

Key
1 housing 7 test sample
2 dish 8 oversize material
3 sieve drum 9 undersize material
4 lid 10 air jet
5 slit-nozzle 11 air discharge
6 sieve 12 pressure gauge socket, with dust hood

Figure 2 — Air-jet sieving apparatus

17
BS EN 196-6:2010
EN 196-6:2010 (E)

5.3 Procedure

If necessary, dry the laboratory sample to constant weight in the oven (5.2.7). Weigh to the nearest 0,01 g
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(25 ± 0,5) g of cement (m). Fit the test sieve with the aperture size e.g 90 µm into the apparatus and transfer
all of the test portion onto the sieve mesh. Take care not to lose any of the test portion.

Fit the lid and switch on the apparatus. Check that the vacuum created is above the minimum value stated in
the manufacturer’s instructions, and that the slit nozzle is rotating properly.

If material adheres to the lid of the apparatus, gently tap the centre of the lid with the mallet.

If the material agglomerates under the action of the air-jet, interrupt the sieving process, and break up the
agglomerates with the soft brush.

After (5,0 ± 0,2) min, switch off the apparatus and carefully remove the sieve. Transfer the material retained
on the sieve into a tray or other suitable container. Carefully clean the mesh of the sieve over the tray using
the soft brush.

Determine the mass of the residue, including the material brushed from the sieve mesh, and record the mass
to the nearest 0,01 g.

Refit the sieve into the apparatus and transfer all of the residue back to the sieve mesh. Repeat the weighing
and sieving stages until the sieving end-point has been achieved, and record the end-point mass to the
nearest 0,01 g. The sieving end-point is defined as being when not more than 0,2 % of the mass of the
original test portion passes through the sieve in 3 min. Express its mass as a percentage, R1 of the quantity
first placed in the sieve to the nearest 0,1 %.

Repeat the whole procedure using a fresh 25 g sample to obtain R2. Then calculate the residue of the cement
R as the mean of R1 and R2 as a percentage, expressed to the nearest 0,01 %.

5.4 Checking the sieve

Sieves should be cleaned and checked for damage after each sieving (e.g. that the mesh is taut and is not
dented or perforated). In addition, check the sieve after every 100 sievings (see 3.4.2).

5.5 Expression of results

The mass retained on each sieve expressed as per cent by mass, m(Pe.g. 63 or 90), (%)), is given by the
following equation:

R × 100
m ( Pe. g .63 or 90 ) = (12)
m

where

m is the mass of the cement in grams (g);

R is the mass of the residue retained on the test sieve in grams (g).

5.6 Repeatability and reproducibility

The precision of the method increases (standard deviation decreases) with the aperture size of the sieve.
Typical values for determination of the residue on a 63 µm sieve are the following:

 The standard deviation of repeatability is 0,1 %;

 The standard deviation of reproducibility is 1,0 %.

18
BS EN 196-6:2010

National Annex NA (informative)


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Material for checking the sieve


For the 'reference material of known (90 µm) sieve residue' (see 3.3) a suitable material in the
UK is B1-30 Quartz5).

National Annex NB (informative)


Method of testing the 'absolute' specific surface of a reference cement
NB.1 Introduction
Since the method specified in clause 4 is 'comparative rather than absolute', there is a need for
a 'reference sample of known specific surface for calibration of the apparatus'. The
determination of the 'known specific surface' calls for an 'absolute' method of determining the
specific surface of a reference cement and this has been given previously in BS 4550. The
procedure has therefore been retained in National Annex NB for the determination of the
'absolute' specific surface of a possible, future reference cement, ideally available from a
European source, for use with this European Standard. Since the method in clause 4 (see
4.5.4) specifies a porosity of 0.500, the former UK procedure has been modified accordingly.

NB.2 Test principle


The fineness is determined from the air permeability of a bed of cement of specified porosity
giving specific surface expressed as total surface area in square metres per kilogram or in
square centimetres per gram.

NOTE This method is a particular form of the general Lea and Nurse constant flow rate air permeability
method described in Appendix B of BS 4359-2:1982.
NB.3 References
The titles of the publications referred to in Annex NB are as follows:

BS 4359-2, Determination of the specific surface of powders. Recommended air permeability


methods

BS 4518, Specification for metric dimensions of toroidal sealing rings ('O'-rings) and their
housings

5
For information on the availability of B1-30 Quartz write to BSI British Standards Customer Services, BSI 389
Chiswick High Road, London W4 4AL or contact cservices@bsigroup.com
BS EN 196-6:2010

NB.4 Apparatus
NB.4.1 Permeability cell, consisting of a metal (stainless steel) cylinder, made in two flanged
parts which are bolted together, containing a perforated plate on which is supported a
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medium filter-paper (Whatman no. 40 or similar) 32 mm in diameter. The joint between the
flanges is rendered airtight by means of a rubber or other suitable gasket. The permeability
cell is provided with a plunger by means of which the cement sample is formed, as described
below, into a cylindrical bed supported by the filter paper.

The essential dimensions are given below:

Internal diameter of upper part of cylinder D = 25.00 ± 0.03 mm


or
D = 25.40 ± 0.03 mm

External diameter of plunger D − 00..05


08 mm

Depth of bed space when plunger is fully 10.00 ± 0.03 mm


inserted

Depth of recess in lower part of cylinder +0


1.6 − 0.03 mm

Thickness of perforated plate + 0.03


1.6 −0 mm

The perforated plate is a push fit in the recess. A typical cell is shown in Figure NB.16).

NB.4.2 Manometers. The permeability cell is to be connected to a bed manometer and a


flowmeter manometer as shown in Figure NB.2. The arms of the bed manometer and of the
flowmeter are about 600 mm long. The capillary tube of the flowmeter has a bore of not less
than 0.5 mm and its dimensions are such that the flowmeter constant C (as defined in NB.5.2)
is between 20 x 10-12 and 40 x 10-12 in the appropriate units. The liquid in both U-tubes is
kerosine (paraffin oil).
The necessary airflow may be produced by any convenient means, but the air entering the
apparatus is to be dried by passing through a tower packed with a suitable desiccant, e.g.
silica gel.

NB.4.3 Balance, capable of weighing up to at least 10 g that can be read to the nearest 0.001
g to an accuracy of ± 0.005 g.

6
The depth of bed space shown in Figure NB.1 is 0.03 mm greater than 10.00 mm in order to allow for the filter
paper which is compressed where it is held by the walls of the metal cylinder but not in the cell itself.
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Figure NB.1 — Details of typical permeability cell


BS EN 196-6:2010
BS EN 196-6:2010
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Figure NB.2 — Typical permeability apparatus with manometer and flowmeter

NB.5 Preparation
NB.5.1 Checking of the dimensions of the permeability cell
Check the dimensions of the cell when the apparatus is received, and after every 50
determinations, by suitable means. The depth of the bed space may be conveniently measured
by using a test piece of hardened steel, of diameter D - 0.2 mm and (10.10 ± 0.03) mm deep
to simulate the cement bed. Place the test piece on the filter paper in the cell, insert the
plunger and check with a feeler gauge that the gap between the shoulder of the plunger and
the top of the cell is (0.10 ± 0.03) mm.

NB.5.2 Determination of the flowmeter constant


NB.5.2.1 General
Check the flowmeter constant every three months by either the method of NB.5.2.2 or
NB.5.2.3.
BS EN 196-6:2010

NB.5.2.2 Collection of air over kerosine


Pass dry air through the flowmeter at a constant rate for a measured time interval. Collect the
issuing air over kerosine and measure its volume. Note the flowmeter reading and calculate
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the flowmeter constant C from the equation:

where
V is the volume (in ml) of dry air passed;
η is the viscosity (in N s/m2) of air at the calibration temperature;
t is the time (in s) during which air is collected;
h2 is the flowmeter reading (in mm);
ρL is the density (in kg/m3) of the kerosine at the calibration temperature.

The viscosity of air in N s/m2 at temperatures in the range of 15 °C to 25 °C is shown below


multiplied by 106.

Temp. °C 15 17 19 21 23 25
to to to to to
16 18 20 22 24
Viscosity 17.8 17.9 18.0 18.1 18.2 18.3

NB.5.2.3 Bubble flowmeter


Measure the flowrate, V/t, using a previously calibrated bubble flowmeter. In order to correct
for the effect of water vapour pressure on the measured flowrate, V should be obtained from:

where
V is the volume (in ml) of dry air passed;
V' is the volume (in ml) of saturated air passed;
P is the atmospheric pressure at the time of test;
PV is the water vapour pressure at the temperature of test.

Note the flowmeter reading and calculate the flowmeter constant C using the equation
in NB.5.2.2.

NB.5.2.4 Replicate determination


Repeat the determination of flowmeter constant for five flowmeter readings over the range
150 mm to 550 mm. Calculate the average value of C and express the result to the nearest 0.1
x 10-12 in the appropriate units.

NB.5.3 Calculation of the apparatus constant


Calculate the value of k for each apparatus as follows and express the result to the
BS EN 196-6:2010

nearest 103 m-1:


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where
ε is the porosity, i.e. 0.500 (see NB.6);
A is the area (in mm2) of the cement bed;
L is the depth (in mm) of the cement bed;
C is the flowmeter constant.

For the cells made to the alternative dimensions specified in NB.4.1:

D = 25.00 mm 25.40 mm

A = 490.9 mm2 506.7 mm2

L = 10.00 mm 10.00 mm

6.94 7.05
k =
C C

NB.5.4 Assembling and testing of the apparatus


Change the filter paper after not more than five determinations. In assembling the
permeability cell ensure that the two parts are firmly bolted together and test the cell and its
connections for leakage.

NOTE This is best done by disconnecting at the manometer the rubber tube leading from the lower end of the
cell, sealing the tube with a screw clip, applying air pressure until the manometer shows a difference in level of
at least 500 mm and then sealing off the air inlet. The reading of the manometer should not change by more than
0.5 mm in a period of 1 min.
NB.6 Procedure
Select a mass of cement from Table NB.1 for a 25.00 mm cell or from Table NB.2 for a
25.40 mm cell which, when compacted, will give a porosity of 0.500 at the measured density
of the cement. (The porosity is defined as the ratio of the volume of pore space to the total
volume of the bed.) Weigh the cement to the nearest 0.001 g and brush it into the
permeability cell, which is gently shaken from side to side to level off the surface. If the
cement is lumpy it may first be rubbed gently with a spatula on glazed paper.
Compact the contents by allowing the cell to fall four times from a height of about 10 mm on
to the bench. Next, slowly insert the plunger and push it home so that the shoulder of the
plunger is in contact with the top of the permeability cell. Do not twist the plunger while in
contact with a cement surface but slowly withdraw it with a twisting motion.

If, on inspection, the cement bed is seen to be disturbed, knock the sample out and repeat the
operation with a fresh sample.

Insert the upper bung and slowly turn on the air; next insert the lower bung slowly and
carefully in order to avoid forcing air through the cement in the wrong direction. Adjust the
BS EN 196-6:2010

rate of airflow until the flowmeter manometer shows a difference in level of 200 mm to 500
mm. When the levels are constant, indicating that steady conditions have been obtained, take
readings of the difference in level h1 of the bed manometer and of the difference in level h2 of
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the flowmeter manometer. Repeat these observations at an airflow rate giving a flowmeter
manometer difference of at least 50 mm from the original rate and within the above range.
NB.7 Calculation
NB.7.1
Calculate the specific surface, Sw, to the nearest m2/kg for each airflow rate from the
equation:

where
k is the apparatus constant determined in accordance with NB.5.3;
ρ is the density (in kg/m3) of the cement determined in accordance with National Annex
NC;
h1/h2 is the ratio of the manometer readings determined in accordance with NB.6.

Where the difference between the two values of Sw is not greater than 5 m2/kg, calculate their
mean and express the result to the nearest m2/kg.

Where the difference between the two values of Sw is greater than 5 m2/kg, repeat the test at a
third airflow rate within the range given in NB.6 to obtain a third value of Sw. If any one of
these three values now lies more than 5 m2/kg from either of the other two, discard it and
calculate the mean of the two remaining values to the nearest m2/kg. Otherwise calculate the
mean of all three values to the nearest m2/kg.

Where there are no two values lying within 5 m2/kg of each other, repeat the complete
procedure with another sample.
NB.7.2
To calculate the specific surface, Sw, to the nearest 10 cm2/g, take the mean value obtained
for Sw according to NB.7.1 and multiply by 10.

Table NB.1 — Mass of cement (in g) required to form a bed 25.00 mm in diameter and
10.00 mm deep having a porosity of 0.500, over density range 2 500 kg/m3 to 3 290 kg/m3

Density 0 10 20 30 40 50 60 70 80 90
kg/m3
2 500 6.136 6.160 6.185 6.210 6.234 6.259 6.283 6.308 6.332 6.357
2 600 6.381 6.406 6.430 6.445 6.480 6.504 6.529 6.553 6.578 6.602
2 700 6.627 6.651 6.676 6.700 6.725 6.750 6.774 6.799 6.823 6.848
2 800 6.872 6.897 6.921 6.946 6.970 6.995 7.019 7.044 7.069 7.093
2 900 7.118 7.142 7.167 7.191 7.216 7.240 7.265 7.289 7.314 7.339
3 000 7.363 7.388 7.412 7.437 7.461 7.486 7.510 7.535 7.559 7.584
3 100 7.609 7.633 7.658 7.682 7.707 7.731 7.756 7.780 7.805 7.829
3 200 7.854 7.879 7.903 7.928 7.952 7.977 8.001 8.026 8.050 8.075
BS EN 196-6:2010

Table NB.2 — Mass of cement (in g) required to form a bed 25.40 mm in diameter and
10.00 mm deep having a porosity of 0.500, over density range 2 500 kg/m3 to 3 290 kg/m3
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Density 0 10 20 30 40 50 60 70 80 90
kg/m3
2 500 6.334 6.359 6.385 6.410 6.435 6.461 6.486 6.511 6.537 6.562
2 600 6.587 6.613 6.638 6.663 6.689 6.714 6.739 6.765 6.790 6.815
2 700 6.841 6.866 6.891 6.917 6.942 6.968 6.993 7.018 7.043 7.069
2 800 7.094 7.119 7.145 7.170 7.195 7.221 7.246 7.271 7.297 7.322
2 900 7.347 7.373 7.398 7.423 7.449 7.474 7.499 7.525 7.550 7.575
3 000 7.601 7.626 7.651 7.677 7.702 7.727 7.753 7.778 7.803 7.829
3 100 7.854 7.879 7.905 7.930 7.955 7.981 8.006 8.031 8.057 8.082
3 200 8.107 8.133 8.158 8.183 8.209 8.234 8.259 8.285 8.310 8.335

NB.8 Reporting
NB.8.1
When reporting in units of m2/kg, report the specific surface to the nearest 1 m2/kg.
NB.8.2
When reporting in units of cm2/g, report the specific surface to the nearest 10 cm2/g.

National Annex NC (informative)


Method of testing cement for density
NC.1 Test principle
The density of cement is determined by displacement of a non-reactive liquid in a
pyknometer.

Methods based on displacement by gas may be used provided that they can be shown to give
the same results.
NC.2 References
The title of the publication referred to in Annex NC is as follows:

BS ISO 3507, Laboratory glassware. Pyknometers


NC.3 Displacement liquid
The displacement liquid is redistilled kerosine (paraffin oil), the density of which should not
change by more than 0.0005 g/cm3 when evacuated for a period of 5 h at a pressure
less than 2.5 kPa (25 mbar).

NOTE A suitable liquid can be prepared in the laboratory by redistilling kerosine and collecting the fraction
condensing at 200 °C to 240 °C. Alternatively, petroleum fractions with boiling ranges within the range 190 °C
to 255 °C and with sufficiently stable density characteristics are commercially available7).

7
For information on the availability of suitable petroleum fractions write to BSI British Standards Customer
Services, BSI, 389 Chiswick High Road, London W4 4AL or contact cservices@bsigroup.com
BS EN 196-6:2010

NC.4 Apparatus
NC.4.1 Pyknometer, of nominal capacity 50 ml conforming to BS ISO 3507.
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NC.4.2 Small funnel, to fit inside the neck of the pyknometer.


NC.4.3 Balance, capable of weighing up to at least 100 g to an accuracy of ± 0.0005 g.
NC.4.4 Thermostatically controlled water bath, capable of being maintained to within ± 0.2
°C at a selected operating temperature slightly above room temperature.

NOTE A convenient operating temperature is 25 °C, but this is left to the discretion of the operator.
NC.4.5 Vacuum desiccator and pump, capable of reducing the pressure to less than 2.5 kPa
(25 mbar).

NOTE A glass vacuum desiccator should be enclosed in a suitable protective mesh guard.
NC.5 Procedure
NC.5.1 General
The water bath (NC.4.4) should be maintained at the same selected operating temperature
throughout the following tests.
NC.5.2 Determination of density of displacement liquid
The procedure should be as follows:

a) Clean and dry the pyknometer and stopper and weigh to ± 0.0005 g.

b) Fill the pyknometer with de-aerated distilled or de-aerated deionized water at room
temperature and, without using undue force, insert the stopper with a slight twist, care being
taken to avoid trapping air bubbles.

c) Immerse the pyknometer nearly to the top of its neck in the water bath and leave for at
least 30 min.

d) After ensuring that air bubbles are absent and that the pyknometer is filled to the top of the
capillary bore, remove with dry filter paper any water on the top of the neck of the
pyknometer where stopper and neck meet, and dry the sides and the top of the stopper, taking
care not to withdraw any water from the capillary.

e) Remove the pyknometer from the water bath and, after allowing it to cool for a few
minutes, wipe it free of water with the minimum of handling, and weigh to ± 0.0005 g.

f) By topping up the pyknometer with more distilled or deionized water, re-immersing it in


the water bath and proceeding as before, make two additional weighings of the pyknometer
filled with water.

g) Calculate the mean of these three weighings, and from the difference between this mean
weighing and the first weighing of the pyknometer and stopper alone, calculate the mass, W1,
of water to fill the bottle at the selected operating temperature.

h) Clean and dry the pyknometer and stopper used in the above test and reweigh to
BS EN 196-6:2010

± 0.0005 g. Repeat the above procedure, but filling the pyknometer with the displacement
liquid instead of water, and determine the mass, W2, (average of three weighings) of
displacement liquid to fill the pyknometer at the selected operating temperature.
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Calculate the density of the displacement liquid to the nearest 0.0005 g/cm3 from the formula:

where

PL is the density (in g/cm3) of displacement liquid at the selected operating temperature;
Pw is the density (in g/cm3) of pure water at the selected operating temperature
(see Table NC.1);
W1 is the mass (in g) of water to fill the pyknometer at the selected operating temperature;
W2 is the mass (in g) of displacement liquid to fill the pyknometer at the selected operating
temperature.

Table NC.1 — Density of pure water, Pw

Temperature Pw
°C g/cm3
18 0.9986
19 0.9984
20 0.9982
21 0.9980
22 0.9978
23 0.9976
24 0.9973
25 0.9971
26 0.9968
27 0.9965
28 0.9963

NC.5.3 Determination of density of cement


Using the procedure described in NC.5.2, calibrate at intervals each pyknometer and stopper
by determining the mass, W3, (average of three weighings) of the pyknometer, stopper and
displacement liquid to fill the pyknometer at the selected operating temperature.

a) Clean and dry the calibrated pyknometer and stopper and weigh to ± 0.0005 g.

b) Place an 8 g to 10 g representative sample of cement in the pyknometer by means of the


small funnel, reweigh with stopper to ± 0.005 g and, from the difference between the first and
second weighings, calculate the mass, W4, of the sample of cement in the pyknometer.

c) Add sufficient displacement liquid to cover the cement sample and half fill the pyknometer
ensuring that the cement is thoroughly wetted by swirling the contents gently, care being
taken to keep cement particles clear of the neck of the pyknometer.
BS EN 196-6:2010

d) Place the pyknometer together with a small beaker containing some displacement liquid, in
the vacuum desiccator and evacuate at a pressure of less than 2.5 kPa (25 mbar) for at least
30 min until bubbles of air cease to be evolved.
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e) Remove the pyknometer from the desiccator and fill with displacement liquid from the
beaker.

f) Using exactly the same procedure as described in NC.5.2, determine the mass, W5,
(average of three weighings) of the pyknometer, stopper, cement sample and displacement
liquid to fill the pyknometer at the selected operating temperature.
NC.6 Calculation
NC.6.1
Calculate the density of the sample of cement to the nearest 0.001 g/cm3 from the formula:

where

P is the density of cement (in g/cm3);


PL is the density (in g/cm3) of displacement liquid at the selected operating temperature;
W3 is the mass (in g) of pyknometer, stopper and displacement liquid to fill the
pyknometer at the selected operating temperature;
W4 is the mass (in g) of sample of cement;
W5 is the mass (in g) of pyknometer, stopper, cement sample and displacement liquid to
fill the pyknometer at the selected operating temperature.

Make two separate determinations on different portions of the sample of cement (if desired
two calibrated pyknometers may be used). If the two results differ by more than 0.02 g/cm3
discard the results and make two fresh determinations.
NC.6.2
Calculate the density of the sample of cement to the nearest kg/m3 by taking the result
obtained at NC.6.1 and multiplying by 1 000.
NC.7 Report
NC.7.1
When reporting in units of g/cm3, report the individual results to the nearest 0.001 g/cm3 and
the average density to the nearest 0.01 g/cm3.
NC.7.2
When reporting in units of kg/m3, report the individual results to the nearest 1 kg/m3 and the
average density to the nearest 10 kg/m3.

National Annex ND (informative)


Reporting of results for density and specific surface
BS EN 196-6:2010

ND.1 Density
This standard specifies in 4.5.3 that the density shall be recorded (mean of the two
determinations) 'to the nearest 0.01 g/cm3'. National Annex NC gives the option of reporting
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in units of g/cm3 (to the nearest 0.01 g/cm3) or, by multiplying by 1 000, in units of kg/m3 (to
the nearest 10 kg/m3). The latter is preferred in the UK.
ND.2 Specific surface (fineness)
ND.2.1
This standard specifies in 4.10 that the specific surface shall be reported (mean of four air
flow times) 'to the nearest 10 cm2/g'. National Annex NB gives the option of reporting the
'absolute' specific surface of a reference cement in units of m2/kg (to the nearest 1 m2/kg) or,
by multiplying by 10, in units of cm2/g (to the nearest 10 cm2/g). The former is preferred in
the UK for all measurements of specific surface.
ND.2.2
The identification of the 'reference cement of known specific surface' should be reported.

National Annex NE (informative)


Cross-references

Publication referred to Corresponding British Standard


ISO 383:1976 BS 572:1985, Specification for interchangeable conical ground
glass joints
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BS EN
196-6:2010
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