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Methods of testing
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cement
Part 6: Determination of fineness
ICS 91.100.10
National foreword
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English Version
Méthodes d'essai des ciments - Partie 6: Détermination de Prüfverfahren für Zement - Teil 6: Bestimmung der
la finesse Mahlfeinheit
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.
© 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.
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:
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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4
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.
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 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
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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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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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
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.
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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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.
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.
4.1 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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EN 196-6:2010 (E)
Dimensions in millimetres
G
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J
4
H
5
L
6 K
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)
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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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
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.
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.
4.5.1 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.
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.
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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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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To give a cement bed of porosity e = 0,500 weigh a quantity of cement, m1, calculated from
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.
4.6.1 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
η is the viscosity of air at the test temperature taken from Table 1, in Pascal seconds (Pa·s).
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.
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 %.
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.
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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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.
4.7.1.2.1 Apparatus
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 %.
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.
where
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
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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 );
η0 is the air viscosity at the mean of the three temperatures, in Pascal seconds (Pa·s) (Table 1).
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:
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.
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
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EN 196-6:2010 (E)
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);
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).
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.
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)
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.
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
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.
5.2.5 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.
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
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 %.
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).
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
R is the mass of the residue retained on the test sieve in grams (g).
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:
18
BS EN 196-6:2010
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 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 perforated plate is a push fit in the recess. A typical cell is shown in Figure NB.16).
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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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.
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.
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
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.
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.
D = 25.00 mm 25.40 mm
L = 10.00 mm 10.00 mm
6.94 7.05
k =
C C
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.
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:
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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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.
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.
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
a) Clean and dry the calibrated pyknometer and stopper and weigh to ± 0.0005 g.
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
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.
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.
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