IS : 4031( Part 3 ) - 1888

Indian Standard

( Reaffirmed 1995 )

METHODS OF
PHYSICALTESTSFORHYDRAULICCEMENT
PART 3 DETERMINATION OF SOUNDNESS

First Revision )
Third
Reprint DECEMBER 1996
(

UDC

66694 : 62017

@I Copytight1988

BUREAU
MANAK

Gr 2

OF

BHAVAN,

INDIAN

STANDARDS

9 BAHADUR SHAH
NEW DELHI 110002

ZAFAR

MARC:
October 1988

IS : 4031 ( Part

3) - 1988

Indian Standard
METHODS OF
PHYSICAL TESTS FOR HYDRAULIC
PART

DETERMINATION

0.

FOREWORD
of individual tests.
Further, since publication
of the original standard in 1968, a number of
standards covering the requirements of different
equipment used for testing of cement, a brief
description
of which was also covered in the
standard, had been published. In this revision,
therefore, reference is given to different instrument specifications deleting the description
of
the instruments, as it has been recognized that
reproducible and repeatable test results can be
obtained only with standard testing equipment
capable of giving desired level of accuracy. This
part covers determination
of soundness by
Le-Chatelier
method and autoclave test.

0.1 This Indian

Standard
( Part 3 ) ( First
Revision ) was adopted by the Bureau of Indian
Standards on 24 February 1988, after the draft
finalized by the Cement and Concrete Sectional
Committee
had been approved by the Civil
Engineering Division Council.
0.2 Standard
methods of testing cement are
essential adjunct to the cement specifications.
This standard in different parts lays down the
procedure for the tests to evaluate physical properties of different types of hydraulic cements.
The procedure for conducting
chemical tests
of hydraulic
cement is covered in IS : 40321985.

0.4 For the purpose of deciding

whether a
requirement
particular
of this standard
is
complied with, the final value, observed
or
calculated,
expressing the result of a test or
analysis, shall be rounded off in accordance tiith
IS : 2-1960*.
The number of significant places
retained in the rounded off value- should be the
same as that of the specified value in this
standard.

0.3 Originally
all the tests to evaluate
the
physical properties of hydraulic cements were
covered in one standard but for facilitating
the
use of this standard and future revisions it has
been decided to print the different
tests as
different parts of the standard and, accordingly
this revised standard has been brought out in
thirteen parts. This will also facilitate updating
*Method of chemical analysis of hydraulic

(Jirst revision ) .

cement

*Rules for rounding off numerical values ( rcoiscd).

f 2C. The relative humidity
shall be 65 f 5 percent.

1. SCOPE
1.1 This standard
( Part 3 ) covers the procedures for determining the soundness of cement.
AND

SELECTION

AND

OF TEST

4. GENERAL
4.1 Soundness of cement may be determined by
two methods, namely Le-Chatelier
method and
autoclave method as described in 5 and 6.
5. LE-CHATELIER

HUMIDITY

of sampling hydraulic

METHOD

5.1 Apparatus
5.1.1 The apparatus for conducting the LeChatelier test shall conform to IS : 5514-1969..

3.1 The temperature of the moulding room, dry

materials and water shall be maintained at 27
*Methods

of the laboratory

3.2 The moist closet or moist room shall be

maintained at 27 f 2C and at a relative humidity of not less than 90 percent.

2.1 The samples of the cement shall be taken in

accordance with the requirements
of IS : 3535
1986* and the relevant standard specification
for the type of cement being tested. The representative sample of the cement selected as above
shall be thoroughly mixed before testing.
3. TEMPERATURE

OF SOUNDNESS

First Revision )

2. SAMPLING
SPECIMEN

CEMENT

*Specification for apparatus used in IkChatdiu

cements (first rcuirion).

tat.

IS : 4031 ( Part 3 ) - 1988

5.1.2 Balance -- The balance
the following re:luirements:

shall

conform

to

being performed.
Cover the mould with another
piece of lightly oiled glass sheet, place a small
weight on this covering glass sheet and immediately submerge
the whole assembly in water at a
temperature
of 27 f 2C and keep there for
24 hours.

On balance
in use, the permissible
variation
at a load of 1 000 g shall be plus or minus 10 g.
The permissible
variation
on new balance
shall be one-half of this value. The sensibility
reciprocal
shall be not greater
than twice
the permissible
variation.

5.2.2 Measure
the distance
separating
the
indicator
points to the nearest 05 mm. Submerge the mould again in water at the temperature
prescribed
above.
Bring
the water
to
boiling, with the mould kept submerged,
in 25
to 30 minutes,
and keep it boiling
for three
hours. Remove the mould from the water, allow
it to cool and measure the distance between
the
indicator
points. The difference
between
these
two measurements
indicates
the expansion
of
the cement.

NOTE 1 - The
sensibility
*reciprocal
is generally
defined as the change in load required to change the
position of rest of the indicating element or elements of
a non-automatic
indicating
scale a definite amount at
any load.
NOTE 2 - Self-indicating
accuracy may also be used.

balance

with

equivalent

5.1.3 Weights - The permissible

variations
weights in use in weighing
the cement shall
as prescribed
in Table 1.
TABLE

WEIOHT

on
be

5.3 Calculation
- Calculate
the mean of two
values to the nearest 05 mm to represent the
expansion of cement.

PERMISSIBLE VARIATIONS
ON WEIGHTS

5.4 Retest - In the event of cement

failing to
meet the test for soundness,
a retest may be
made after aeration.
For this purpose,
spread
out the cement in a layer of 75 mm thickness
and store it for 7 days in an atmosphere
maintained at 27 f 2C and relative humidity of 50
to 80 percent.
Retest this cement
as described
in 5.2.

PERMISSIBLE
VARIATION
ON
WEIGHTS
IN
USE, PLUS OB

MINUS
g

(1)

(2)

500

035

300

030

250

025

200

020

100

015

50

010

20

005

10

004

003

002

001

6. AUTOCLAVE
6.1 Apparatus
6.1.1 Balance
6.1.2

Procedure

Same

as 5.1.2.

Weights -

Same

as 5.1.3.

6.1.4 MouldsMoulds
of 25 X 25 mm size
and 282 mm internal length and other accessories
conforming
to IS : 10086-1982*.

5.2.1 Place the lightly oiled mould on a lightly

oiled glass sheet and fiil it with cement
paste
formed by gauging cement with 078 times the
water
required
to give a paste of standard
consistency
[see IS : 4031 (Part 4)-1988*].
The
paste shall be gauged in the manner and under
the conditions
prescribed
in IS : 4031 (Part 4 )1988*, taking
care to keep the edges oi the
mould gently together
while this operation
is
*Methods of physical tests for hydrualic
cement:
4 Determination
of consistency of standard cement
( jirt revision )

6.1.3 Graduated
Glass
Cylinders - Graduated
glass cylinders
of 150 ml capacity
shall be used.
Th e permissible
variation
on these cylinders
shall be plus or minus one millilitre.
The main
graduation
lines of the cylinders
shall be in
circles and shall be numbered.
The least graduations shall extend
at least one-seventh
of the
way around, and intermediate
graduations
shall
extend
at least one-fifth of the way around the
cylinder.
The graduation
lines may be omitted
for the lowest 5 ml.

5.1.4 Water Bath-Water

bath
capable
of
containing
immersed
Le-Chatelier
moulds with
specimens and of raising their temperature
from
27 f 2C to boiling in 27 f 3 minutes.
5.2

METHOD

6.1.5 Autoclave - The autoclave

shall consist
of a high pressure steam boiler equipped
with
suitable safety device. The capacity
of heating
unit shall be such that with maximum
load
( water
plus specimens ) the pressure
of the
saturated
steam in the autoclave
may be raised

Part
paste

*Specification for moulds for use in tests of cement

concrete.

and

IS : 4031 ( Part 3 ) - 1988

to a gauge pressure of 21 MPa or to an absolute
pressure
of about 22 MPa,
in 1 to 1) hour
from the time the heat is turned
on.
The
automatic
pressure control shall be capable
of
maintaining
the pressure
at 21 f 01 MPa
corresponding
to a temperature
of 2157 f
17C. The autoclave
shall be designed to permit
the pressure to drop from 21 MPa to less than
007 MPa in one hour after the heat supply has
been shut off. It shall be equipped
with a vent
valve for allowing the escape of air during the
early part of the heating period and for releasing
any steam pressure remaining
at the end of the
one-hour
cooling period.
The pressure
gauge
shall have a nominal
dial diameter
of 115 mm
and shall be graduated
from 0 to 41 MPa with
scale division of not more than 004 MPa. The
error in the gauge shall not exceed plus or minus
002 MPa at the operating
pressure of 21 MPa.
6.1.6 Length Comparator - Changes in length of
the test specimen
shall be measured
by an
apparatus
conforming
to IS : 9459-1980.
6.2 Preparation

of Test

Specimens

6.2.1 Preparation of Moulds - The moulds shall

be thinly covered
with mineral
oil. After this
operation,
the stainless steel or non-corroding
metal
reference
inserts with knurl heads shall
be set to obtain
an effective
gauge
length
of
250 mm, care being taken to keep them clean
and free from oil.
6.2.2 Mixing Cement Paste - The standard batch
of cement paste shall consist of 500 g of cement,
mixed with sufficient
water to give a paste of
standard
consistency.
6.2.3 Moulding Specimens - Immediately
follothe
completion
of mixing,
the
test
wing
specimens shall be moulded in one or two layers,
each layer being compacted
With the thumb or
forefinger
by pressing the paste into the corners,
around
the reference
inserts,
and along the
surfaces
of the moulds
until a homogeneous
specimen
is obtained.
After the top layer
has
been compacted,
the paste shall be cut off flush
with
the top of the mould
and the surface
smoothed
with a few strokes of the trowel.
During the operations
of mixing and moulding,
the hand shall be protected
by rubber gloves.

6.3.1 At 24 f Q h after moulding,

the specimens shall be removed
from the moist atmosphere, measured
for length,
and placed in the
autoclave
at room temperature
in a rack so that
the four sides of each specimen shall be exposed
to saturated steam. The autoclave
shall contain
enough water to maintain
an atmosphere
of
saturated
steam
vapour
during
the
entire
period oftest.
Ordinarily,
7 to 10 percent of the
volume of the autoclave
shall be occupied
by
water.
6.3.2 To permit air to escape from the autoclave during the early portion
of the heating
period,
the vent valve shall be left open until
steam begins to escape ( see 6.4 ). The valve shall
then be closed and the temperature
of the autoclave shall be raised at such a rate as will bring
the gauge pressure of the steam to 21 MPa in 1
to 1) h from the time the heat is turned on. The
21 f 01 MPa pressure shall be maintained
for
3 h.
At the end of 3 hours period,
the heat
supply shall be shut off and the autoclave
cooled
at a rate such that the pressure will be less than
01 MPa at the end of the hour, and any pressure
remaining
shall be slow released
by partially
opening the vent valve until atmospheric
pressure
is attained.
The autoclave
shall then be opened
and the test specimens
immediately
placed in
water, the temperature
of which is above 90C.
The water surrounding
the bars shall then be
cooled at a uniform
rate by adding cold water
so that the temperature
of the water shall be
lowered to 27 f 2C in 15 min. The water surrounding
the specimens shall then be maintained
at 27 f 2C in 15 min when the specimens
shall
be surface-dried
and their lengths
measured
again.
6.4

Safety

Precautions

6.4.1 The
pressure
gauge
should
have
a
maximum
capacity
of 42 MPa. This is important because with too small a capacity
there is
but a little length of arc in which the gauge
hand may indicate pressure above the specified
maximum
working pressure. The operator
must
be sure that the gauge hand has not passed the
maximum
graduation
on the scale.
6.4.2 It is well to leave the pressure
gauge
tested,
but in any
event
thermometer
shall
always be used together with the pressure gauge,
so as to provide a means of detecting any failure
of the pressure gauge to operate
properly
and
also to indicate
any unusual conditions
such as
that resulting from loss of water from the autoclave during the test.

6.2.4 Storage of Test Specimen - After the mould

has been filled, it shall be immediately
placed
Specimens
in a moist closet or a moist room.
shall remain
in the moulds in the moist room
for at least 24 h.
If removed
from the moulds
before
24 h, they shall be kept in the moist
closet or moist room until tested.
*Specification
of length change
concrete.

6.3 Prooedure

6.4.3 The
automatic
control
tained in proper working order

for apparatus
for use in measurement
of hardened cement paste, mortar and

6.4.4
relieve
3

The safety
the pressure

shall be mainat all times.

valve shall be set so as to

at about 6 to 10 percent

18:4031(Part3)-1988
above the maximum
of 21 MPa specified,
that
is at about 23 MPa. The safety valve shall be
tested at least twice a year, either with a gaugetesting device or by adjusting
the automatic
controls so as to allow the autoclave
to reach a
pressure of about 23 MPa at which pressure the
safety valve shall either open or be adjusted to
open. The safety vaive discharge shall be directed away from the operator.
NOTE - Unexpected
combinations
of conditions may
really occur. For example, in one case the automatic
control had failed, the safety valve had stuck, and the
gauge hand, wluch at first- glance appeared to be at
about zero. had reallv oassed the maximum graduation
and had come to stop on the wrong side of the pin. This
condition
of the gauge was finally detected
and the
pressure,
then of an unknown magnitude,
was released
before failure could occur in the apparatus.

6.4.5 Heavy leather work gloves shall be worn

to prevent burning of the hands when removing
the top of the autoclave
at the end of the test.
The vent valve shall be directed
away from the
operator.
When removing
the autoclave lid, the
lid shall be so tilted that any steam escaping from
beneath
the lid may be discharged
away from
the operator.
Care shall be taken to avoid scalding by any liquid that may have been used in
the autoclave
well.
6.4.6

It shall

be remembered

that

for many

of the autoclave pressure gauges now in use, the

return of the gauge hand to the initial rest or
starting point does not necessarily
indicate
zero
pressure within the autoclave;
there may then
still remain an appreciable
pressure.
6.4.7 A few drops of kerosene
placed in the
vent valve about once a week will aid in keeping
the needle clean and in good-working
condition.
6.5 Calculations
- The difference
in lengths
of the test specimen before and after autoclaving
shall be calculated
to the nearest 001 percent of
the effective gauge length which is the length
between the innermost points of the metal inserts
used as reference
points and shall be reported
as the autoclave
expansion
of the cement.
A
contraction
( negative expansion ) shall be indicated by prefixing a minus sign to the percentage
expansion reported.
6.6 Retests - In the event of cement failing to
meet the test for soundness,
a retest may be
made after aeration.
For this purpose,
spread
out the sample in a layer of 75 mm thickness
and store it for 7 days in an atmosphere
maintained at 27 f 2C and relative
humidity
of 50
to 80 percent.
Retest this cement as described
in 6.2 and 6.3.

Bureau of Indian Standards

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AMENDMENT

NO. 1 MARCH 1993

TO
IS 4031( Part 3 ) : 1988 METHODS OF PHYSICAL
TESTS FOR HYDRAULIC
CEMENT
PART 3 DETERMINATION

OF SOUNDNESS

( First Revision )
( Page 2, clause 5.1.4 ) -Substitute

the following

for the existing clause:

51.4 Water Bade - Water bath with means of heating, capable of containing
immersed Le-Chatelier moulds with specimens and of raising their temperature
from 27 + 2C to boiling in 27+ 3 minutes.

(CED2)
Printed at Printograph, New Delhi (INDIA).