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IS 5623 (2012): Glass - Determination of Co-efficient of

Linear Thermal Expansion [CHD 10: Glassware]

“!ान $ एक न' भारत का +नम-ण”

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 IS 5623 : 2012
ISO 7991 : 1987

Hkkjrh; ekud
dk¡p — eè; js[kh; rkih; çlkj xq.kkad Kkr djuk
( nwljk iqujh{k.k )

Indian Standard
GLASS — DETERMINATION OF COEFFICIENT OF
MEAN LINEAR THERMAL EXPANSION
( Second Revision )

ICS 81.040.01

© BIS 2012
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

August 2012 Price Group 4

Glass, Glassware and Laboratoryware Sectional Committee, CHD 10

NATIONAL FOREWORD

This Indian Standard (Second Revision) which is identical with ISO 7991 : 1987 ‘Glass — Determination
of coefficient of mean linear thermal expansion’ issued by the International Organization for
Standardization (ISO) was adopted by the Bureau of Indian Standards on the recommendation of the
Glass, Glassware and Laboratoryware Sectional Committee and approval of the Chemical Division
Council.

This standard was first published in 1970 and then subsequently revised in 1999 to bring it in line with
the latest version of ISO 7991 : 1987. During this revision, the Committee felt that it would be more
convenient to prepare this standard by adoption of ISO 7991 on dual number basis.

The text of ISO Standard has been approved as suitable for publication as an Indian standard without
deviations. Certain conventions are, however, not identical to those used in Indian Standards. Attention
is particularly drawn to the following:

a) Wherever the words ‘International Standard’ appear referring to this standard, they should
be read as ‘Indian Standard’.
b) Comma (,) has been used as a decimal marker while in Indian Standards, the current
practice is to use a point (.) as the decimal marker.

In this adopted standard, reference appears to certain International Standards wherein the standard
atmospheric conditions to be observed are stipulated which are not applicable to tropical/subtropical
countries. The applicable standard atmospheric conditions for Indian conditions are 27 ± 2°C and
65 ± 5 percent relative humidity and shall be observed while using this standard.

In this adopted standard, reference appear to the following International Standard for which Indian
Standard also exists. The corresponding Indian Standard, which is to be substituted in its place, is
listed below along with its degree of equivalence for the edition indicated:

International Standard Corresponding Indian Standard Degree of Equivalence

IEC 584-1 Thermocouples — Part 1: IS 10625 : 1983 Reference tables for Technically Equivalent
Reference tables nickel/chromium-copper/nickel
(chromel-constantan) thermocouples

The technical committee has reviewed the provision of the following International Standard referred
in this adopted standard and has decided that its is acceptable for use in conjunction with this
standard:

International Standard Title

ISO 7884-8 Glass — Viscosity and viscometric fixed points — Part 8: Determination
of (dilatometric) transformation temperature

For the purpose of deciding whether a particular requirement of this standard is complied with, the
final value, observed or calculated, expressing the result of a test, shall be rounded off in accordance
with IS 2 : 1960 ‘Rules for rounding off numerical values (revised)’. The number of significant places
retained in the rounded off value should be the same as that of the specified value in this standard.
 IS 5623 : 2012
INTERNATIONAL STANDARD ISO
ISO 7991
7991 : 1987
: 1987 (E)

Indian Standard
GLASS — DETERMINATION OF COEFFICIENT OF
MEAN LINEAR THERMAL EXPANSION
Glass - Determination ( Second
of coefficient
Revision )of mean linear
thermal expansion

1 Scope and field of application For the purposes of this International Standard, the nominal
reference temperature, to, is 20 OC; therefore the coefficient of
This International Standard specifies a method for determining mean linear thermal expansion is denoted by a(20 OC; t).
the coefficient of mean linear thermal expansion of glass in the
elastic solid-like state, well below the transformation tempera-
ture (see ISO 7884-8). .
4 Apparatus
This International Standard applies to all glasses of normal
bulk-production compositions. lt does not apply to fused silica, 4.1 Device for measuring the specimen length, to an ac-
glass ceramics or other glasses of similarly low linear thermal curacy of 0,l %.
expansion coeff icients.
4.2 Push-rod dilatometer, capable of determining changes
in length of the specimen of 2 x 10V5 l. (i.e. 2 Fm per
2 References
100 mm).
ISO 7884-8, Glass - Viscosity and viscometric fixed Points -
The contact forte of the extensometer should not exceed 1 N.
Part 8: Determination o f fdila tome tric) transforma tion tem-
That forte shall act through contacts of planes with spherical
pera ture.
faces the radii of curvature of which shall be not less than the
rod diameter of the specimen. In some special assemblies (sec
IEC Publication 584-1, Thermocouples - Part 7: ßeference
figure 1) parallel planes are needed.

The specimen-holding assembly shall ensure that the specimen

is held firmly in Position and shall prevent even small changes in
3 Definition
its alignment with respect to the push-rod axis throughout the
test (sec examples given in the annex).
For the purposes of this International Standard, the following
definition applies.
If the specimen-holding assembly is made of vitreous silica, see
the precautions given in 7.2.
coefficient of mean linear thermal expansion, a(t,; t) : The
ratio of the Change in length of a specimen within a
From time to time, a Performance test shall be carried out using
temperature interval to that temperature interval, related to the
a reference material (see clause 8).
initial specimen length.

lt is given by the following equation: 4.3 Furnace, compatible with the dilatometer assembly, for
temperatures up to 50 OC above the expected transformation
temperature. The working Position of the furnace relative to the
1 1 - 10
a(t,; t) = 7 x - . . . (1) dilatometer assembly shall be defined with a repeatability sf
t - to
0 0,5 mm in both the axial and the radial directions.
where
Within the range of testing temperatures (i.e. up to tempera-
tures about 150 OC below the highest expected transformation
f0 is the initial or reference temperature;
temperature, t9, and at least up to 300 OC), the furnace shall be
capable of marntaining a constant temperature to + 2 OC over
t is the actual (constant or variable) specimen tem-
the whole specimen length.
perature;

l. is the length at temperature t. of the specimen of glass 4.4 Furnace control device, suitable for the desired rate of
under test (usually a rod made from the glass); increase in temperature up to (5 + 1) OC/min within the test
range (sec 6.1) and for a cooling rate of (2 + 0,2) OC/min for
I is the specimen length at temperature t. the annealing procedure according to 5.2.

1
1
IS
ISO5623
7991: 2012
: 1987 (E)
ISO 7991 : 1987
4.5 Temperature-measuring device (e.g. a thermocouple
of type E, J or K in accordance with IEC 584-11, capable of
determining the temperature of the specimen to + 2 OC in the
temperature range between t. and t.
5 Test specimen
5.1 Shape and size
The test specimen is usually in the form of a rod. Its shape
depends on the type of dilatometer used. The length l. shall be
at least 5 x IO4 times the resolution of the dilatometer’s
measuring device for the Change in length.
NOTE - The specimen may be, for example, a rod either with a cir-
cular Cross-section having a diameter of 5 mm or with a Square cross-
section 5 mm x 5 mm, and between 25 and 100 mm in length. In cer-
tain cases, a Cross-section of at least 100 mm2 is more convenient (sec
the annex).
5.2 Preparation
The test specimen shall be annealed before the test by heating
it to about 30 OC above the transformation temperature and
then cooling it to about 150 OC below the transformation
temperature at a rate of (2 + 0,2) OC/min, followed by further
cooling to room temperature in draught-free air.
5.3 Number
The test shall be carried out with two test specimens (sec also
7.4).
6 Procedure
6.1 Choice of the test range
In accordance with clause 3, the nominal reference temperature
is 20 OC. For practical reasons, however, the measurement may
be started between 18 and 28 OC. The preferred final actual
temperature is 290 OC < t < 310 OC. If this is not practical,
then the alternative values 190 OC G t < 210 OC, or, in special
cases, 95 OC < t < 105 OC or 390 OC < t < 410 OC may be
Chosen. The corresponding nominal values of t are 300 OC,
200 OC, 100 OC, and 400 OC, respectively.
All readings of temperatures and temperature differentes shall
be taken with an accuracy to 2 OC. Though these actual values
are used in the calculations in accordance with clause 7, the
test range shall be expressed in terms of the nominal tem-
peratures (see 7.4). For a given coefficient a(20 OC; t) ex-
pressed in terms of the nominal temperature, no influence on
the value of the coefficient tan be detected within the limits
specified for the preferred actual temperatures.
6.2 Determination of the reference length
Determine the reference length Z. of the annealed specimen
(sec 5.2) to an accuracy of 0,l % at the reference temperature
to. Subsequently insert the specimen into the dilatometer and
22
wait for about 5 min before beginning the test as described in
6.3 or 6.4.
6.3 Test at increasing temperature
Determine the Position of the dilatometer at the initial
temperature t. and take this reading as zero for the uncorrected
Change in length, AImeas, which will be measured. Subse-
quently set the furnace control device (4.4) to the desired
heating Programme and Start the Programme. Record the
temperature t and the related Change in length AI,,,, until the
desired final temperature has been reached.
NOTE - The rate of temperature increase should not exceed
5 OC/min.
As the dilatometer readings of AI,,,ea,are recorded during the
increase in the temperature between t. and t (values Chosen in
accordance with 6.11, it should be borne in mind that a
temperature differente will exist between the hot junction of
the thermocouple and the test specimen; therefore a correction
shall be applied to the apparent temperature of the test
specimen.
NOTE - The magnitude of this correction depends on the rate of
temperature Change and the rate of heat exchange between the fur-
nace and the test specimen. lt is essential that the correction is deter-
mined experimentally by comparison with measurements at constant
temperatures.
64. Test at constant temperature
Determine the Position of the dilatometer at the initial
temperature t. and take this reading as zero for the uncorrected
Change in length, Almeas, which will be measured. Subse-
quently heat the furnace to the selected final temperature t and
hold it constant to + 2 OC for 20 min. Then take from the
dilatometer reading the value of AZ,,,,.
NOTE - Although the test at increasing temperature (6.3) enables a
set of coefficients a(t,; t) with various values of t to be determined in
one test run, the test at constant temperature (6.4) should be preferred
if only one final value of t is required since this test affords the better
precision.
7 Expression of results
7.1 Calculation of the final length
From the measured Change in length, Al,eas, the corrected
length I at temperature t is calcu lated using the following equa-
tion :
I = Z. + AZ,,,, + AZQ - AIB . . . (2)
where the correction terms AI0 and AZBare explained in 7.2
and 7.3 respectively.
7.2 Calculation of the expansion of the specimen-
holding assembly
In the case of a simple push-rod dilatometer, the correction
ter *rn AlQ in equation (2) is the thermal expansion of that part of
 IS 5623: :1987
ISO7991 2012(El
ISO 7991 : 1987

the specimen-holding assembly alongside the specimen, hav- The measurements on glass and the blank test shall be carried
ing the length I, at temperature tO. out under identical conditions. The blank test shall be repeated
at least whenever a Performance test in accordance with
In the case of a differential push-rod dilatometer, the correction clause 8 is carried out.
term AZ0 is the expansion of a reference rod with the specimen
length Z0at temperature fO. 7.4 Calculation of the coefficient of mean linear
thermal expansion
In either case, the correction term AZ0 is calculated using the
following equation In Order to calculate the coefficient of mean linear thermal ex-
pansion, ab,; t), insert the measured values of I, and Almeas,
Al0 = \* l aQ l (t - t,)

the corrections established in accordance with 7.2 and 7.3, and

the actual values of & and t (with t corrected, if it is determined
where ao is (in the case of a simple push-rod dilatometer) the using the test at increasing temperature) into the following
coefficient of mean linear thermal expansion of the material equation :
from which the specimen-holding asembly is made or (in the
case of a differential push-rod dilatometer) the coefficient of
mean linear thermal expansion of the material of the reference 1 A/ meas + ‘AlQ - AzB
ab,; t) = - X . . . (4)
rod. lo t - to

If specimen-holding assemblies, push-rods or reference rods

are made from vitreous silica which is essentially hydroxyl-free, Calculate a(20 OC; 300 OC), a(20 OC; 200 OC), a(20 OC; 100 OC)
the values of aQ given in the table may be used. Before these or a(20 OC; 400 OC) for the two test specimens (5.3) to two
Parts of the dilatometer are used for the first time, they shall be significant figures if a(20 OC; t) < 10 x 10-6 K -1 or to three
annealed for 7 h at 1 100 OC, and then cooled from 1 100 to significant figures if a(20 OC; t) > 10 x 10-6 K-1.
900 OC at a constant rate of 0,2 OC/min.
If the results for the two test specimens differ by not more than
In Order to avoid devitrification of vitreous silica the surfaces 0,2 x 10-” K-l, take the arithmetic mean. If the differente is
shall be kept clean. lt is recommended that they are cleaned larger, repeat the test with two other test specimens.
twice with analytical-grade alcohol, after which contact with
bare fingers shall be avoided.
Performance test
Table - Coefficient of mean linear th expansion aQ In Order to check that the whole test device is functioning cor-
for vitreous silica rectly, the test procedure and calculation laid down in clauses 6
and 7 shall be carried out on a specimen of a reference material,
I Range of temperature, OC Value of aQ, K-l the value of the coefficient of mean linear thermal expansion of
20 to 100 0,54 x IO-6 which is certified. l)
20 to 200 0,57 x IO-6
20 to 300 0,58 x IO-6 Recommended reference materials are as follows :
20 to 400 0,57 x IO-6
- vitreous silica annealed according to 7.2;
NOTE - The values of aQ given in the table are altered if the System is
heated to above 700 OC.
- sapphire Single crystal;

- chemically pure platinum.

7.3 Determination of the dilatometer
The dilatometer correction term AIS is needed mainly because
of irregularities in temperature distribution within the transient
range between the specimen at temperature t and the exten-
someter at ambient temperatures. The dilatometer correction
term should be determined by means of a blank test.
In the case of a simple push-rod dilatometer, the specimen-for
the blank test is made of the same material as the dilatometer. If
that material is vitreous silica, the specimen for the blank test
shall be annealed in accordance with 7.2.
In the case of a differential push-rod dilatometer , two identical
specimens of any suitable material tan be used.
correction
NOTE - Sintered alumina (Al203) as a reference material is very insen-
sitive to the thermal treatment applied in the test procedure laid down
in this International Standard. However, the values of the mean linear
thermal expansion coefficient differ from one rod to another.
The shape and dimensions of the reference specimen shall be
similar to those of the specimens usually tested in the test
device.
Care shall be taken to ensure that the thermal expansion
behaviour of the reference material is not altered by the test. If
the reference material is a glass, it shall be annealed (or re-
annealed) in accordance with 5.2, unless other procedures are
specified by the certifier.

1) Enquiries about sources of certified reference materials (CRMs) may be addressed to the S ecretariat of REMCO, Inter ,national Organization for
Standardization (ISO), 1, rue de Varembe, Case postale 56, CH-121 1 Geneva 20, Switzerland

3
3
IS
ISO5623
7991: 2012
: 1987 (E)
ISO 7991 : 1987

9 Test report e) type of test run konstant or in perature,

rate of increase)
The test report shall include the following information: fl coefficient of rnean linear thermal expansion a(20 OC; t)
exP ressed in IO-6 K-1
reference to this International Standard;
- to two significant figures, if a(20 OC; t) < 10 x IO-6
b) specification, type and state of delivery of the glass K-1;
tested ;
- to three significant figures, if a(20 OC; t) > 10 x IO-6
Cl shape, size and number of test specimens; K-L

d) type of push-rod dilatometer used; For the temperatures t. and t, use the nominal values (sec 7.4).

4
 ISO7991
IS 5623 :: 1987
2012(EI
ISO 7991 : 1987

Annex

Devices for self-adjusting alignment of specimen and push-rod axis

(This annex forms an integral part of the Standard.)

ldeally the axes of the test specimen and push-rod coincide,
and the length I, should lie in the same axis. In practice, small
deviations between the axes of the test specimen and push-rod
may occur. Such deviations are negligible only when that
misalignment remains constant throughout the test. Similar
considerations hold true for the push-rod direction and the
working direction of the extensometer. Changes in alignment
(e.g. caused by Vibration of the apparatus) shall be avoided by
appropriate devices as shown in the examples (figures 1
and 2).
An example for minimizing changes in alignment in a
dilatometer assembly working almost vertically is illustrated in
figure 1. The guiding devices made from platinum wire prevent
further lateral changes in the Position of specimen and push-
rod once the stable Position is achieved by slight shaking. The
axial movements caused by thermal expansion, however, are
not hindered. Exactly vertically mounted dilatometer
assemblies have been found to be the most sensitive with
respect to changes in alignment during the test.

5
IS 5623 : :2012
ISO7991 1987 (E)
ISO 7991 : 1987

Guiding device, before bending

1 Specimen-holding tube with dilatometer base and sealed end plug ground flat perpendicular to tube axis, made from fused silica
2 Push-rod made from fused silica
3 Guiding device for the push-rod, made from platinum wire, 0,5 to 1 mm in diameter
4 Guiding device for the specimen, made from platinum wire, 0,5 to 1 mm in diameter

NOTE - Between the base and the push-rod, half the tube is tut away so that the test specimen tan be easily changed.

Figure 1 - Example of a specimen-holding and push-rod assembly of a dilatometer working almost ver tically

6
 IS 5623
ISO 7991 ::1987
2012(EI
ISO 7991 : 1987

An example for minimizing changes in alignment in a distance holders. The push-rod is also supported by two
dilatometer working horizontally is illustrated in figure 2. The spheres of suitable diameter guided on the same guide-rod.
support for the specimen consists of four spheres (e.g. made After the apparatus has been shaken gently the test specimen
from ruby or fused silica), a cylindrical guide-rod, and suitable and push-rod achieve a stable Position.

1 Specimen-holding tube with dilatometer base made from fused silica

2 Push-rod made from fused silica
3 Distance holders made from fused silica
4 Supporting spheres made from fused silica or ruby
5 Guide-rod made from fused silica

NOTE - Between the base and the push-rod, half the tube is tut away so that the test specimen tan be easily changed.

Figure 2 - Example of a specimen-holding and push-rod assembly of a dilatometer working horinontally

7
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This Indian Standard has been developed from Doc No.: CHD 10 (1786).

Amendments Issued Since Publication

______________________________________________________________________________________
Amendment No. Date of Issue Text Affected
______________________________________________________________________________________
______________________________________________________________________________________
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