ISO 9597:2008
(Main)Cement — Test methods — Determination of setting time and soundness
Cement — Test methods — Determination of setting time and soundness
ISO 9597:2008 specifies the methods for determining standard consistence, setting times and soundness of cements. ISO 9597:2008 applies to common cements and to other cements and materials, the standards for which call up this method. It might not apply to other cement types that have, for example, a very short initial setting time. The method is used for assessing whether the setting time and soundness of a cement is in conformity with its specification. ISO 9597:2008 describes the reference methods and allows the use of alternative procedures and equipment, as indicated, provided that they have been calibrated against the reference methods. In the event of a dispute, only the reference equipment and procedures described in ISO 9597:2008 can be used, excluding any alternatives.
Ciments — Méthodes d'essais — Détermination du temps de prise et de la stabilité
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Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 9597
Second edition
2008-11-15
Cement — Test methods —
Determination of setting time and
soundness
Ciments — Méthodes d'essais — Détermination du temps de prise et
de la stabilité
Reference number
ISO 9597:2008(E)
©
ISO 2008
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ISO 9597:2008(E)
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ISO 9597:2008(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Principles. 1
4 Laboratory, equipment and materials. 1
5 Standard consistence test . 2
6 Setting time test. 5
7 Soundness test . 7
Annex A (informative) Alternative method for setting time tests. 10
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ISO 9597:2008(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 9597 was prepared by Technical Committee ISO/TC 74, Cement and lime.
This second edition cancels and replaces the first edition (ISO 9597:1989), the following clauses and
subclauses of which have been technically revised, based on comments received by the secretariat.
⎯ 4.1: Requirement for the laboratory relative humidity is reduced to a minimum of 50 % from a minimum of
65 %.
⎯ 4.2.5: Drinking water is permitted for storing and boiling test specimens; drinking water is no longer
permitted in the production of paste since such water varies in quality between places and even with time
in the same laboratory.
⎯ 5.1: The Vicat mould is permitted to have a cylindrical, in addition to truncated conical, shape.
⎯ 5.2.1: The time permitted for scraping paste from the sides and bottom of the mixing bowl is increased
from 15 s to 30 s.
⎯ 5.2.3: The end-point for the determination of standard consistence is increased to (6 ± 2) mm from
(6 ± 1) mm.
⎯ Clause 6: The determination of the setting time is carried out whilst the specimen is immersed in water.
⎯ 6.1.1: In the determination of the setting time, the use of automatic apparatus conforming to the
requirements of the reference method is permitted.
⎯ 6.1.3: In the determination of the setting time, the tolerance on storage temperature for specimens is
reduced to (20,0 ± 1,0) °C from (20 ± 1) °C.
⎯ 6.2.2: The end-point for the determination of the initial setting time is increased to (6 ± 3) mm from
(4 ± 1) mm.
⎯ 6.3.1: It is required to confirm the end-point for the determination of the final setting time by testing at two
additional positions in the test specimen.
⎯ 7.1.1: The material for the construction of the Le Chatelier apparatus to determine the soundness is
extended to any non-corrodible spring metal.
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ISO 9597:2008(E)
⎯ 7.1.3: The minimum relative humidity in which specimens for determination of soundness are stored is
reduced to 90 % from 98 %.
⎯ 7.2: The determination of soundness is carried out once.
⎯ 7.4: Where a retest of the determination of soundness is required, the relative humidity at which the
cement sample is stored is reduced to 50 % from 65 %.
⎯ Annex A: An alternative method for testing the setting times of slow-setting cements is included.
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INTERNATIONAL STANDARD ISO 9597:2008(E)
Cement — Test methods — Determination of setting time and
soundness
1 Scope
This International Standard specifies the methods for determining standard consistence, setting times and
soundness of cements.
The method applies to common cements and to other cements and materials, the standards for which call up
this method. It might not apply to other cement types that have, for example, a very short initial setting time.
The method is used for assessing whether the setting time and soundness of a cement is in conformity with its
specification.
This International Standard describes the reference methods and allows the use of alternative procedures and
equipment, as indicated, provided that they have been calibrated against the reference methods. In the event
of a dispute, only the reference equipment and procedures described in this International Standard can be
used, excluding any alternatives.
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.
ISO 679, Cement — Test methods — Determination of strength
3 Principles
Cement paste of standard consistence has a specified resistance to penetration by a standard plunger. The
water required for such a paste is determined by trial penetrations of pastes with different water contents.
The setting time is determined by observing the penetration of a needle into cement paste of standard
consistence until it reaches a specified value.
The soundness is determined by observing the volume expansion of cement paste of standard consistence as
indicated by the relative movement of two needles.
4 Laboratory, equipment and materials
4.1 Laboratory
The laboratory in which specimens are prepared and tested shall be maintained at a temperature of
(20 ± 2) °C and a relative humidity of not less than 50 %.
A laboratory temperature of (25 ± 2) °C or (27 ± 2) °C may be maintained in warm countries, provided the
temperature is stated in the test report.
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ISO 9597:2008(E)
The temperature and relative humidity of the air in the laboratory and the temperature of the water in the
storage containers shall be recorded at least once per day during working hours.
Cement, water and apparatus used to make and test specimens shall be at the laboratory temperature.
NOTE See Annex A for storage conditions applied when testing setting times by an alternative method.
Where temperature ranges are given, the target temperature at which the controls are set shall be the middle
value of the range.
4.2 Equipment and materials
4.2.1 General requirements
The tolerances shown in Figures 1 and 2 are important for the correct operation of the equipment in the
testing procedure. When regular control measurements show that the tolerances are not met, the equipment
shall be rejected, adjusted or repaired. Records of control measurements shall be kept.
Acceptance measurements on new equipment shall cover mass, volume and dimensions to the extent that
these are indicated in this International Standard, paying particular attention to those critical dimensions for
which tolerances are specified.
In those cases when the material of the equipment can influence the results, the material is specified and shall
be used.
The approximate dimensions shown in the figures are provided as guidance to equipment manufacturers or
operators. Dimensions that include tolerances are obligatory.
4.2.2 Balance, capable of weighing to an accuracy of ± 1 g.
4.2.3 Graduated cylinder or burette, capable of dispensing to an accuracy of ± 1 ml.
4.2.4 Mixer, conforming to ISO 679.
NOTE A more homogeneous paste is produced at the lower limit of tolerance for the clearance between the blade
and the bowl.
4.2.5 Water, distilled or deionized, shall be used for making the specimens.
Drinking water may be used for storing and boiling specimens.
4.2.6 Timer, capable of measuring to an accuracy of ± 1 s.
4.2.7 Ruler, capable of measuring to an accuracy of ± 0,5 mm.
5 Standard consistence test
5.1 Apparatus
Use the manual Vicat apparatus as shown in Figure 1 a) and 1 b) with the plunger as shown in Figure 1 c).
The plunger shall be of non-corrodible metal in the form of a right cylinder of at least 45 mm effective length
and of (10,00 ± 0,05) mm diameter. The total mass of moving parts shall be (300 ± 1) g. Their movement shall
be truly vertical and without appreciable friction, and their axis shall coincide with that of the plunger.
The Vicat mould [see Figure 1 a)] to contain the paste under test shall be of hard rubber, plastics or brass. It
shall be of cylindrical or preferably truncated conical form (40,0 ± 0,2) mm deep and shall have an internal
diameter of (75 ± 10) mm. It shall be adequately rigid and shall be provided with a base-plate larger than the
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ISO 9597:2008(E)
mould and at least 2,5 mm thick, constructed of impermeable material resistant to attack by cement paste,
e.g. plane glass.
Moulds of other metal may be used, provided that they are of the specified depth and that their use has been
calibrated against the specified mould.
It is recommended that a laboratory uses base-plates of equal thickness so that it is necessary only to adjust
the scale of the Vicat apparatus once for several determinations.
Dimensions in millimetres
a) Side view with mould in an upright position for b) Front view with mould inverted for final
initial setting time determination setting time determination
Figure 1 (continued)
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ISO 9597:2008(E)
Dimensions in millimetres
c) Plunger for standard d) Needle for initial set e) Needle with attachment for
consistence final set
Key
1 mould 5 water
2 correcting weights 6 air vent (∅ – 1,5)
3 base-plate 7 air vent
4 container
a
View from below needle with attachment for determining final setting time.
NOTE Only one correcting weight is required for each Vicat apparatus if the mass of the plunger and the needles with
and without the attachment is always the same, e.g. (9,0 ± 0,5) g.
Figure 1 — Typical manual Vicat apparatus for determination of standard consistence and setting time
5.2 Procedure
5.2.1 Mixing the cement paste
Weigh, to an accuracy of ± 1 g, by means of the balance (4.2.2), 500 g of cement and a quantity of water, e.g.
125 g. When water is measured by volume using the graduated cylinder or burette (4.2.3), it shall be
dispensed to an accuracy of ± 1 ml. Mix each batch of paste mechanically using the mixer (4.2.4). The timing
of the various mixing stages refers to the times at which mixer power is switched on/off and shall be
maintained within ± 2 s. Proceed as follows.
a) With the mixer in the operating condition, place the water and cement into the bowl, taking care to avoid
loss of water or cement; complete the addition within 10 s.
b) Immediately start the mixer at low speed whilst starting the timing of the mixing stages. In addition, record
the time to the nearest minute as “zero time”.
NOTE “Zero time” is the point from which the initial (see 6.2) and final (see 6.3) setting times are calculated.
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ISO 9597:2008(E)
c) Stop the mixer after 90 s for 30 s during which time detach, by means of a suitable rubber or plastics
scraper, all the paste adhering to the wall and bottom part of the bowl and place it in the middle of the
bowl.
d) Restart the mixer and run at low speed for a further 90 s. The total mixer running time shall be 3 min.
Any other mixing method may be used, provided that it has been calibrated against the reference method.
5.2.2 Filling the mould
Transfer the paste immediately to the lightly oiled mould, which has previously been placed on the lightly oiled
base-plate, and fill it to excess without undue compaction or vibration. Remove any voids in the paste by
gently tapping the slightly overfilled mould against the ball of the hand. Remove the excess by a gentle sawing
motion with a straight-edged implement in such a way as to leave the paste filling the mould and having a
smooth upper surface.
NOTE Some oils have been found to affect the setting time test; mineral-based oils have been found to be suitable.
WARNING — Wet cement paste is highly alkaline and can cause skin burns. Avoid direct contact with
skin during manual operations by wearing protective gloves.
5.2.3 Determination of standard consistence
Adjust the manual Vicat apparatus with the plunger [Figure 1 c)], attached in advance of the test, by lowering
the plunger to rest on the base-plate being used and adjusting the pointer or the scale to read zero. Raise the
plunger to the stand-by position. Immediately after levelling the paste, transfer the mould and base-plate to the
Vicat apparatus and position it centrally under the plunger. Lower the plunger gently until it is in contact with
the paste. Pause in that position for between 1 s and 2 s in order to avoid initial velocity or forced acceleration
of the moving parts. Then release the moving parts quickly and allow the plunger to penetrate vertically into
the centre of the paste. The release of the plunger shall occur 4 min ± 10 s after zero time. Read the scale at
least 5 s after penetration has ceased or 30 s after the release of the plunger, whichever is the earlier.
Record the scale reading, which indicates the distance between the bottom face of the plunger and the
base-plate, together with the water content of the paste expressed as a percent mass fraction of the cement.
Clean the plunger immediately after each penetration.
Repeat the test with pastes containing different water contents until one is found to produce a distance
between plunger and base-plate of (6 ± 2) mm. Record the water content of that paste to the nearest 0,5 % as
the water for standard consistence.
6 Setting time test
6.1 Apparatus
6.1.1 General
The apparatus described in 6.1.2 to 6.1.5 is that used in carryi
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