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“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 13411 (1992): Glass reinforced polyester dough moulding


compounds (DMC) [PCD 12: Plastics]

“!ान $ एक न' भारत का +नम-ण”


Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”


है”

Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
( Reaffirmed 2003 )

Indian Standard
GLASS REINFORCED POLYESTER DOUGH
MOULDING COMPOUNDS-SPECIFICATION

UDC 678’674‘046’364 - 404’9

0 BIS 1992

BUREAU OF INDIAN STANDARDS


MANAK BIIAVAN, 9 BAHADtJR SHAH ZAFAR MAR@
NEW DELHI 110002

November 1992 Price Group 12


Plastics Sectional Committee, PCD 12

FOREWORD

This Tndian Standard was adopted by the Bureau of Indian Standards, after the draft finalized bv
the Plastics Sectional Committee had been approved by the Petroleum, Coal and Related Products
Division Council.

Although phenolic and amino moulding powders remain by far the most commonly used
thermosetting moulding composirion. a number of new materials have been introduced based on
polyesters, epoxides, and silicone resins. Five classes of polyester compound may be recognized:

a) Dough Mouldiog Compound ( DMC ), also known as Bulk Moulding Compounds ( BMC );
b) Sheet Moulding Compound ( SMC );
c) Alkyd Moulding Compositions sometimes referred to as ‘Polyester Alkyds’;
d) Diallyl Phthalate Compounds; and
e) Diallyl Iso-Phthalate Compounds

Glass reinforced polyester moulding compounds have in general a high mechanical strength and also
good etectrical insulation and arc resistance. In view of this, these are suitable for many engineering
applications.

The Dough Moulding Compounds ( DMC ) were originally developed in an attempt to combine the
mechanical properties of polyester glass laminates with the speed of cure of conventional moulding
powders. In spite of their somewhat high cost, they have now established themselves in a number
of applications where a mechanically strong electrical insulant is required.

Dough moulding compositions are prepared by blending resin, powdered mineral filler, reinforcing
fibre, pigments and lubricants, in a dough mixer usually of the Z-blade type. The resins are similar
to conventional laminating resins, a fairly rigid type being preferred so that cured mouldings may
be extracted from the mould at 160°C without undue distortion. Organic peroxide such as benzoyl
peroxide and tertiary butyl perbenzoate are commonly used as catalysts. The choice of catalyst
will influence cure conditions and also will be a f<ictor in whether or not surface cracks appear on
the mouldings. Mmeral fillers such as calcium carbonate are employed not only to reduce costs
but to red,lce shrinkage and to aid the flow since an incorrect viscosity may lead to such faults as
finre bunching and resin-starved area<. Although glass fibre ( E-type ) is most commonly used as
the reinflj:,cing tibre, sisal is used in cheaper compositions. Stearic acid or metal stearates are the
usual lubncants.

In common with all polyester moulding compositions, the dough moulding compounds cure without
evolution of volatiles and thus pressures as low as I’4 MPa, but normally about 6.9 MPa, may be
used. The material of putty like consistency is first preformed into a ball shape and loaded into
the mould of a fast acting press in such a way that there should be a minimum of weld lines and
undesireable fibre alignment. Temperature in the range of 1lO”C-170°C may be employed and
at the higher temperatures cure times of less than one minute per millimetre thickness are possible.

In this standard, three grades of Dough Moulding Compounds are covered and which are further
distinguished according to their electrical and mechanical properties.

Characteristics given in Table 3 are optional and are subject to agreement between the purchaser
and the supplier.

Indian Standard Specilication for Sheet Moulding Compounds, IS 13410 : 1992 is also brought out.

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 or analysis 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 otf value should bc the same as that of the specititd
value in this standard.
IS 13411: 1992

Indian Standard
GLASSREINFORCEDPOLYESTERDOUGH
MOULDINGCOMPOUNDS-SPECIFICATION
1 SCOPE and size, Section2 Determinationof
density of solid plastics
1.1 This standard specifies requirements for
8543 (Part 41 Methods of testing plastics: Part 4
themlosetting polyester dough mouldingcompounds
Set 1) : 1984 Short term mechanical properties,
which are classified according to their electrical and
Section 1 Determination of tensile
mechanical properties and which are used for
properties
processing by moulding-transfer, compression and
injection. 11320 : 1985 Glass fibre rovings for the
reinforcement of polyester and of
1.2 Compounds whose fibrous reinforcement include epoxide resin systems
glass, other than&glass, are excluded in this standard.
13360 Plastics - Methods of testing:
2 REFERENCES (Part 1) : 1992 Part 1 Introduction
13360 (Part 6/ Plastics - Methods of testing:
The following Indian Standards are necessary Set 6) : 1992 Part 6 Thermal properties, Section 6
adjuncts to this standard: Determination of flammability by
oxygen index
IS No. Title
3 TERMINOLOGY
2824 : 1975 Method for determining compara-
tive tracking index of solid 3.1 For the purpose of this standard, the definitions
insulating materials under moist given in IS 2828 : 1964 and the following shall apply.
conditions (first revision )
2828 : 1964 Glossary of terms used in the plastic 3.1.1 Batch
industry
A quantity of material so designated by the supplier
3396 : 1979 Methods of test for volume and and substantially uniform in quality.
surface resistivities of solid electrical
insulating materials (first revision ) 3.1.2 E-Glass
4486 : 1967 Recommended methods for the
LOW alkali glass containing not more than 1 percent
detemlination of the pemtittivity and alkali metal oxides expressed as Na,O as prescribed in
dielectric dissipation factor of
IS 11320 : 1985.
electrical insulating materials, at
power, audio and radio frequencies 3.1.3 Dough Motdding Compound (DMCf
including wavelengths
4905 : 1968 Methods for random sampling Homogeneous mixture of resins and chopped rein-
forced fibres with or without fillers, shapeless, capable
6262 : 1971 Method of test for power factor and of being moulded under heat and pressure. High vis-
dielectric constant of electrical cosity is achieved by increased filler contrnt.
insulating liquids
Unsaturated polyester resin systems 3.1.4 Type Tests
6746 : 1972
for low pressure fibre reinforced Tests carried out to prove conformity with the
plastics specification. These are intended to prove the
Guide for determination of thermal general qualities and raw materials of a give11 type of
8504
DMC.
(Part 1) : 1977 endurance properties of electrical
insulating materials: Part 1 Temp-
3.1.5 Acceptcrnce Tests
erature indices and thermal
endurance profiles
Tests carried out on samples taken from a lot I’or 1h(,
8504 Guide for determination of thermal purpose of acceptance of the test.
(Part 2) : 1983 endurance properties of electrical
insulating materials: Part 2 List of 3.1.6 Routine Tests
materials and available tests
Tests carried out at manufacturer’s works on DMC LO
8543 (Part I/ Methods of testing plastics: Part 1 check the requirements which are likely to vary during
Set 2) : 1979 Characteristics of polymer structure production.

1
IS 13411: 1992
4 GRADES b) the processing characteristics in the same
mould in the same machine and under the
4.1 The thermosetting polyester dough moulding same processing conditions are presumed
compounds shall be of the following grades: identical.
D, - General Purpose Grade;
6.4.1 The material characteristics in the moulding,
D, - Mechanical Grade; and namely, thepropertiesofthemoulded material, depend
on the type of moulding material, the production
D, - Electrical Grade. conditions during moulding, the flow of the moulding
material and the connected internal structure in the
4.1.1 The above grades are suitable for moulding by moulding.
compression/transfer processes. EZach of the above
grade if suitable for moulding by injection process NOTE - The requirements given under Tables 1, 2 and 3 are
based on standard test specimen made from the moulding mare-
shall be prefixed with the letter ‘J’ as given below: rial. This information gives an indication of the properties of rhc
moulding.
!?.~clmn/AcJD 1 - General purpose grade suitable
for injection moulding.
6.5 When tested by the appropriate methods, the
moulded and conditioned material shall comply with
4. I .2 Spccirrl Grdcsjbr Spccijic Requiremcn~s
the requirements specified in Tables 1 and 2.
With either improved chemical, thermal, electrical or NOTE-See Table3 for optional requirements Ihal arc subject
mechanical properties, special grades may be derived IO agreement and which a purchaser may wish to specify.
from the above. Such grades shall be as agreed to
between the purchaser and the supplier but shall be 6.6 Resistance to Chemicals
designated with suffix ‘S’ as given below:
The chemicals resistance to outdoor exposure are not
E.wmpl~‘D2S -Modified mechanical grade with included as standard tests. These may be covered
good electrical proprrlies. under optional requirements as agreed to bctwrcn the
purchaser and thr supplier as given in Table 3.
5 COMI’OSITION
6.7 Thermal Endurnnce
5.1 The material shall essentially consists of an un-
saturated polyester resin system generally conforming The endurance behaviour of plastic is susceptible to
to IS 6746 : 1974 combined with fillers and fibrous variations with tcmpcrature. Determination ofthcrmal
reinforcement to form a mix which is pliable at room rating corresponding IO extrapolated lift of 20 OOCI
temperature and is capable of being cured by moulding hours as specified in IS 8.504 (Part 1) : 1977 and IS
under heat and pressure. The reinforcement shall bc K.504 (Part 2) : 1983 has IO be carried out by a series of
glass fihres made out of E-glass. lcsts and is intended to be a guideline for USC as
insulating material.
6 REQIJIREMENTS
Till the industry is able to give the values for thermal
6.1 Colow rating, as an alternative, the maximum coulinuolla
operating tcmpcraturo is specified under optional
The colour of the polycstcr moulding compound shall properties in Table 3.
be as agreed by the purchaser and the supplier.
6.8 Storage Life
6.2 Form
6.8.1 The supplier shall state Ihc sloragc lift of ~hc
The moulding compound shall be in thr dough form.
material in the original unopened container under the
ccinditions recommended by Ihc supplier.
6.3 Processal~ility
Immediatelyafterthefirstopeningofthe~~c~~ltai~~~~rs,i~~
The material shall be suilahle for processing by any time within the stated expiry date 19.2.1(v)] 111(
compression, transfer and/or injection moulding. In material shall be mouldable and shall comply with Ih(
general, the following shall bc the processing requircmcnts stated in 6.
parameters:
7 I’RlW.4RATION OF TEST Sl’li(‘Ihil’NS
a) Temperature : 120” to 160°C
b) Curing Time : 30 to 60 scc!mm thickness 7.1 Mould to siye the tcht pirccx Icqulrctl li)r 111~
dctcrminatiou ofclcctrical blrcngth, walcl abscjrl)ticllr
1.j Pressure : 3 lo IS MPa and cul Itic remaining test picccs I’roni 1hc Itiotildcd
sheet. Howe\,cr, in the case 01‘diqpulc mould 111~irkI
6.4 The requirement for uniformity ot’ a particular pact alrcngth picccs to siyr.
type of material prcsupposcs Ihal:

a) the requirements according to Tablr 1, Tablr


2 and those given in Table 3 (covcrcd in
agreement between the purchaser and the
supplier) arc ail fulfilled; and

2
IS 13411: 1992

8 TESTING 9.2.2 The containers may also be marked with the


Standard Mark.
8.1 The requirements have been classified as per
Type Test, Acceptance Test and Routine Tests. 10 SAMPLING

8.2 The routine tests and acceptance tests shall be 10.1 Lot
carried out for every batch by the supplier.
All the containers of glass reinforced polyester dough
moulding compounds (DMC) of the same grade, pro-
9 PACKING AND MARKING
duced underthe same conditions of manufacture shall
constitute a lot.
9.1 Packing
10.1.1 Each lot shall be tested separately forthe vari-
9.1.1 The polyester dough moulding compounds
ous requirements of the specification. The number of
with a net mass of 25 or 50 kg shall be covered in a
containers to be selected from each lot for this purpose
polyethylene bag and wrapped with cellophane lining.
shall be as given in Table 4.
The material shall be packed in suitable containers.

NOTE - Packing in metallic drums are prone to cause contami- 10.1.2 The containers shall be selected at raudom
nation. from each lot. For this purpose reference may bc made
to IS 4905 : 1968.
9.2 Marking
10.2 Number of Tests
9.2.1 Containers of the material shall be legibly
From each containers selected in the sample, the
marked with indelible ink with the following informa-
number of test specimens shall be moulded from
tion.
different portions in accordance with 7.1. The number
a) Indication of the source of manufacture and of test specimens shall be sufficient to carry out all the
trademark, if any; acceptance and routine tests as given in Tables 1,2 and
3 respectively. The DMC shall also be tested for the
b) Material classification, flow and colour;
thermal endurance as per 6.7.
c) Batch number;
10.3 Criteria for Conformity
d) Date of manufacture;
Any sample failing in one or more requirements of the
e) Date of expiry under the conditions specified specification shall be termed as defective.
by the supplier (which shall not be less than 60
days from the date of manufacture); and No defective shall be found in the lot for the lot to be
accepted as conforming to the specifications.
f) Net mass.

Table 1 Material Requirements for Dough Moulding Compound


( Clauses 6.4,6.4.1 and 6.5 )

Sl Chlu-Pcterlst3a Requirrmeata NPllJIV Methods


No. Of of Test

Grade D, Grade D, Grade D, Test Ref LO

(1) (2) (3) (4) (5) (6) (7)

i) CJlass content, percenr IS 20 20 ‘Type Annex A


by mass, Min

ii) Mould shrinkage linear 0.2 0.2 0.2 ACCf2plNlCC Annex 11

percent, Max

iii) 170 170 170 Acceptance Annex C‘

3
IS 13411: PI92
Table 2 Requirements for Moulded Dough Moulding Compounds
( Clauses 6.4, 6.4.1 nnd 6.5 )

SI Charactel-lstlcs Requirements Nature Methods


NO. of of Test,
-Grade D, Grade D, Grade Dy Test Ref to

(1) (2) (3) (4) (5) (6) (7)

9 Density of moulding, -1.6 to 3.0-‘---+’ Routine IS 8543 (Part l/


glcrnl Set 2) : 197Y

ii) Water absorption, percent, t------- 0.2 - Type Annex D


Mnx

iii) Izod impact 15 20 18 Type Annex B


strengrh (Notched), Acceptance
KJ/mZ, MI’N for D 2

iv) Flexural strength. MPa. Min 60 80 70 Routine Annex F

v) Modulus of elasticity, t 12x 10’ to 15 x 10’ --+ Type IS 8543 (Part 41


MPa Set 1) : 1984

vi) Surface resistivity 1 x 10’0 1 x 101’ 1 x lo’? Rouline IS 3396 : lY7Y


(24 h in waler), ohm,Mi,,

vii) Volume resistivity, 1 x 10’” 1 x 10” 1 x KS* Routine IS 3396 : 1979


ohm-cm, Min

viii) Tracking resistance, CTI, 600 600 1000 Type IS 2824 : 1975
Milt

ix) Power arc resistance, 120 140 180 Type acceptance Annex G
Set, Mitt for D,

x) Dielectric strength at 9oOC 8 8 10 Type IS 6262 : 1971


in oil kV/mm, Min

xi) Dissipation factor 0.03 0.01 Type IS 4486 : 1967


(4-days al 80 percent
RII at 1KHz)

xii) Heat disrortion 125 135 135 Type Annex II


temperature, ‘C, Min

xiii) Oxygen index, percent, 23 25 25 Type IS 1336O(Part 6/


Min Set 6) : 1992
IS 13411 : 1992

Table 3 Optional Requirements for Moulded Dough Moulding Compounds


[ CZnuses6.4.(a), 6.4.1, 6.5, 6.6 and 6.7 ]

Sl Requirements Methods
No. F -Y of Test,
Grade D, Grade D, Grade D, Ref to

(1) (2) (3) (4) (5) (6)

9 Continuous use temperature 120 130 130


(long-term), T, Mar

ii) Resistance to chemicals values IO be agreed kiween the Annex J


purchaser and the supplier
\
iii) Post shrinkage, percent, Max +---0.01 / Annex R

iv) Coefficient of linear thermal + 20 x 10-G-----3 Annex K


expansion, cm/cmPC

Table 4 Scale of Sampling


( Chse 10.1.1 )

Lot Size Number of Containers to be


(Number of Contatners) Selected in P Sample

(1) (2)

up to 100 5
101 to 150 8
151 to 300 13
301 to 500 20
501 to 1 ooo 32
1001 and above 50
IS 13411: 1992

ANNEX A
[Table 1, SZNo. (i) ]

DETERMINATION OF GLASS CONTENT


( Adapted from BS 5734 : Part 1: 1979 )

A-O GENERAL A-4.2 Place the crucible plus test piece on a pipeclay
triangle and ignite over a Bunsen burner until most of
This is a simple method of test that has been shown to the volatile material has been removed. Transfer the
be appropriate for glass-reinforced plastics. If inor- crucible and contents to the muffle furriace at a tem-
ganic fibres other than glass are also present, the perature of 575 + 25OC and maintain at this tempera-
method determines the total reinforcement content. ture until all carbonaceous matter has disappeared.
Cool as previously and weigh. Reheat in the muffle
This method is not suitable when the particle size of
furnace for half an hour, cool and reweigh. Repeat
any acid-insoluble filler is larger than 75 pm.
until the mass is constant to within 0.01 g.
A-l APPARATUS
A-4.3 Transfer the residue into a 500 ml beaker con-
The following apparatus is required. taining approximately 25 ml of distilled water. Add an
excess of 5 M HCl up to a maximum of 25 ml. Agiratc
A-l.1 Spatula the contents gently with a glass rod.

A-l.2 Oven, capable of being thermostatically Where separation of discrete layers of reinforcement
controlled at 105 2 S°C. occurs add 200 ml of distilled water and transfer Ihe
layers to the sieve.
A-l.3 Balance, capable of weighing to an accuracy
of?o.OOlg. Where separation into layers does not occur, mix
gently to a smooth paste and then add 200 ml of
A-l.4 Fused Silica Crucibles, 70 mm diameter. distilled water. Transfer the contents of the beaker to
the sieve.
A-l.5 MutIle Furnace
A-l.6 Bunsen Burner A-4.4 In both cases after transfer to the sieve, wash
with distilled water to remove the filler from Ihe
A-1.7 Desiccator reinforcement, this may be conveniently carried out by
A-l.8 Pipeclay Triangle putting the sieve into a large evaporating basin con-
taining enough distilled water to partly fill the sieve.
A-l.9 Beakers Raising or lowering of the sieve in the water assists the
separation. Dry the sieve and contents at 105 + 5OC and
A-1.10 Acid-Resistant Sieve, of 75 pm nominal transfer the glass to a suitable preweighed container
aperture. (M,) and reweigh (M,).

A-l.11 Glass Rod, fitted with rubber ‘policemen’. A-4.5 Repeat the procedure with the remaining lest
pieces.
A-1.12 Tweezers
A-5 CALCIJLATION AND EXPRESSION Ok
A-2 KEAGENTS RESULTS
Distilled water conforming to IS 1060 and 5 M hydro- A-5.1 Calculate the percentage glass contcnl using
chloric acid (HCl) are required. the following formula:
A-3 TEST PIECES
Percent glass content =
M, -M, x l(X)
Takr a rcprcscntative sample from the material under
MA - M,
trst. Use a minimum of three test pieces each of
approximately 10 g, takingcare to ensure Ihe edges are where
not frayed. M, is the mass of the dry crucible,
A-4 PROCEDITWE M, is the mass of the crucible plus specinlrn.
M, is the mass of the container, and
A-4.1 Clean and dry the silica crucible and ignite for
half an hour in a mufflc-furnace at 575 t 25°C. Allow M, is the mass of the container plus the dry
to cool to belwcT11 1owc and 200°C 011 a clean glass.
pipeclay triangle, and 111rn transfer to the dcsiccakx.
When cool weigh to 0.001 g (M,). Place a test pircr in A-5.1.1 Calculate the arithmetic mean of the three
, crucible and reweigh (MJ. rchulls.
i
6
. IS 13411: 1992

ANNEX B
[Table 1, SZNu. (ii) ]
DETERMINATION OF MOULD SHRINKAGE
[ Adpated from IS0 2577 : 1984 ]

B-O GENERAL 4 for compression moulding - bars of length


120 mm, width 15 mm and thickness 10 mm;
The characteristics moulding shrinkage and the and
shrinkage after heat treatment of thermosetting
moulding materials are useful for the production b) for injection moulding - flat square plaques
approximately 120 mm x 120 mm x 4 nun.
control and for checking uniformity of manufacture
of thermosetting materials. Furthermore, knowledge B-4.2 The specimen shall be moulded to sample by
of the initial shrinkage of thermosetting materials is
compression or injection mouldingusinga mould with
important for the construction of the moulds, and
single or multiple cavities.
knowledge of post shrinkage for establishing the
suitability of the moulding material for the B-5 PROCEDURE
manufacture of moulded pieces with accurate
dimensions. B-5.1 If not already known, measure the lengths of
the cavities (or the distances between the engraved
B-l DEFINITIONS
marks in the mould) to the nearest 0.02 mm at a
temperature of 27 t 2OC. Record these measurements
B-l.1 Moulding Shrinkage
for use in the calculation of shrinkage.
The difference in dimensions between a moulding and NOTE - From time to time, moulds should be checked for wear,
the mould cavity in which it was moulded, both the etc. As an alternate to measuring directly the lengths of the cold
mould and the moulding being at normal temperature moulds, the gauge for the moulds may beobtainedvery precisely
when measured. by cold-moulding specimens from lead and measuring their
lengths.

B-l.2 Post Shrinkage


B-S.2 Mould at least two specimens from the sample
Shrinkage of a plastic product after moulding, during to be tested, under the conditions given below:
post-treatment, storage or use.
For compression moulding:
B-2 APPARATUS Mould the specimens under the conditions of
pressure, temperature, time, etc, specified in
B-2.1 Mould, press, etc, suitable for moulding the test the relevant specification for the material.
specimelti specified in B-4. For compression mould-
ing, a positive or a semi-positive mould with single or In case of those fibrous materials that are to be
multiple cavities shall be used. injection-mouldcd as a plaque, at least four
specimens should be tested.
If required, marks may be engraved in the mould
near opposite ends of the specimen to facilitate the B-5.3 After removal from the mould, allow the, test
accurate measurement of the length of the cavity and specimen to cool to room temperature by placing
them on a material with low thermal conductivity and
the specimens.
underanappropriate load toavoid warping. Store them
NOTE - If multiple cavities are used with a positive mould, at a temperature of 27 + 2°C and a relative humidity of
resulting variations in tesl specimen density may be sufficient to
65 t 2 percent for a period of minimum 88 h, or for
produce inconsistenl shrinkage.
suchshortertime as can be shown to give the same test
B-2.2 Equipment, suitable for measuring the lengths results.
of the test specimen and the corresponding cavity of
B-5.4 Before measuring the lengths of the test
the mould to within 0.02 mm.
specimens, place them on a flat surface or against a
B-2.3 Oven (for Post Shrinkage Only) straight edge in order to determine any warp or
d&r&m. Any test specimen that has a warp exceeding
B-3 SAMPLING 1 percent or its length shall hc discarded.

A reprcscntative sample shall t)c taken from the 11-5.5 For the determination of moulding shrinkage,
umulding material and he kept at room temperature in mrasurc, to the nearest 0.02 mm, the Irngths ol’ tht
air-tight containers, without any conditioning, until bar spcciniens parallel to thrir major axis bctwrcn
rnoulded into test specimrus. opposite cud faces or the distances 1~c1wcc11the
gsugc marks, at a tenlpcraturt ol’27 -C2°C. Mcaxun-
B-4 TEST SPFCIMFNS
, / , Incuts ofplaque specimens shall hc niadc at dislaacc 01’
20 nlnl front tbc corners, two mcasurcmc’nts in t hc
H-4.1 The test specimen shall IX: same direction.
c
7
IS 13411: 1992 .
NOTE - In order to measure the effect of orientation on the B-6 EXPRESSION OF RESULTS
shrinkage of an injection-moulded specimen, shrinkages in two
directions at right-angles (each of which is calculated from an
average of hvo measurements in the same direction) are
B-6.1 The moulding shrinkage (Ns) is given, as a
measured and calculated independently. percentage, by the formula:

B-S.6 For the determination of post-shrinkage, place MS =


Lo-L* x loo
r
the test specimens, measured as described in B-5.5,
in an oven maintained at the temperature given below. where
Support the specimens to avoid deformation and in
such a way that they are separated from each other. Lo is the length, in millimeters, of the dimensions
of the mould, determined as in B-5.1; and
The following temperatures shall be: L, is the length, in millimeters, of the correspond-
ing dimensions measured on the test specimen
1 loo t 3OC for urea-formaldehyde moulding according to B-5.5.
materials; and
NOTE - When shrinkage is determined using injection-
80° 2 2OC for all other thermosetting mould- moulded plaques, L and L, are each the averages of two read-
ing materials. ings, measured in the same direction, taken 20 mm from the
corners of the mould and the lest specimen respectively.

The times of exposure shall be: B-6.2 Post-shrinkage (PS) is given as a percentage, by
the formula:
48 2 1 h for rapid determination; and
L‘ -L2 xl00
168 t 2 h for normal determination. ps4sh
orps16*h
= ,
NOTE - Post-shrinkage depends strongly on the time of expo- where
sure. Therefore, the exposure time should be noted (see B-6.2
and B-7.5) and should be specified in the specification for the L, is as defined in B-6.1; and
material.
L, is the length, in millimeters, of the same dimen-
At the end of the heating period, remove the test specimen from sion of the test specimen, measured after heat
the oven and allow them lo cool in a standard atmosphere of 27 treatment for 48 or 168 h according to B-5.6.
+ 2°C and a relative humidity of 65 + 5 percenl for at least 4 h.
Ni(l1’1.- When post-shrinkage is being determined using
After Ihe cooling period, measure the test specimens again, at a injection-moulded plaques, L, is the average of two readings,
temperature of 27 + 2°C to the nearest 0.02 mm. as specified in measured in the same direction, taken 20 mm from the corners
B-5.5. of Ihe mould and the tesl specimen.

ANNEX C
[Tuhle 1, SI No. (iii) ]
METHOD OF TEST FOR DETERMINATION OF FLOW FOR GLASS REINFORCED
POl.YESTER MOIJLL)ING COMPOUNDS

C-O GENERAI, (:-1 UEFINITlC~N


Polyester moulding compounds have a limited shclf-
I‘IOW
life. Hence, in order to have a consistent quality of
mouldcd c0111p0u11ds throughout its shelf-life,
Thr flou rncasurcd on a disc moulded in a flow
dclrrmination of flow characteristics in a mould is
mould ol’ a material of prcscribcd wcighl uudcl
essenlial. The Cup llow rate mcasurcment for
specified moulding conditions is called ‘Ilow’. 7’hc
phenolic and alkyds moulding malerials arc nol
unit of nitasurcnien1 is uim.
adopted AS these materials have dil’fcrcnt flow
properlies. As Ihe malerial has by nalure au easy Ilow
charackristics, a test similar to ~hcrmoplas~ic has (T-2 AI’l’ARA’l’llS
been dcvclopcd, which is iu pmctirc with
manufaclurcrs of Inaltrials and niouldcr\.

8
IS 13411: 1992

C-3 PREPARATION OF TEST SPECIMEN C-3.5 Ensure that maximumclosingtime ofthe mould
does not exceed 10 seconds.
C-3.1 Draw equal samples from at least 3-bags of not

less than 1.5 kg. C-4 PROCEDURE

C-3.2 Draw 3-samples of 18.5 2 2 g each as charge C-4.1 Mould the discs as per conditions specified
weight for determination of llow property from the above.
1.5 kg sample.
C-4.2 Eject the moulding while hot and allow it to
C-3.3 The ‘test specimen’ shall be in the form of a cool to room temperature.
moulded disc (see Fig. 1) as per the following mould-
ing conditions: C-4.3 Measure the flow length on either side to the
nearest 5 mm on 3-samples.
Pressure, MPa = 5 - 30
C-4.4 The flow in mm is determined by the average of
Temperature, oC = 130 - 160
the 3-samples tested.
Curing time, S/mm = 60
NOTE - t Jse 30 kmnes capacityhydraulic press
C-4.5 The report shall include:
a) Average flow length in mm; and
C-3.4 Place the charge centrally and mould the speci-
IWII in the compression mould. b) Minimum flow length in mm.

ANNEX D
[ Table 2, SI No. (ii) ]

DETERMINATION OF WATER ABSORF’TION

D-0 PRIN(:IPI,E D-l.4 Desiccator

Complete immersion of test specimen of the plastic D-l.5 Means, of measuringdimensions ofspecimens,
material in water for a specified period of time and if rcquircd.
at a specified temperature. Determination of changes
in the mass of the test specimens after immersion in D-2 TEST SPECIMEN
water and if requricd after elimiuation of water by
drying. D-2.1 Three specimens shall be tested. They may be
obtained directly by moulding or by machining. In the
The water absorption may bc expressed in the follow- lattcrcase, thecutsurfaceshallbesmoothandshallnot
i ng ways: show any trace of charring that may be due to the
method of preparation.
a) As the mass of water absorbed,
D-2.2 The test specimen shall bc 50 2 1 mm square
h) As the mass of water absorbed per unit of
and a thickness of 3 t 0.2 IIIIIL It shall be moulded
surface arca, and under the conditions given in 7.1 (or under the condi-
c) As a pcrccntage by mass of water absorbed tions prescribed by the suppliers of the material).
with respect to the mass of the test specimen.
D-3 PROCEDURE
D-l API’AKA’l’l1S D-3.1 General Conditions

D-1.1 Dalanre, with an accuracy of 1 mg. D-3.1.1 The volume of water used shall be at least
8 ml per square centimetre of the total surface of the
D-l.2 Oven, capable of being controlled at SO + 3°C test specimen, so as to avoid any extraction product
or at auy other agreed Icmpcraturc. becoming excessively concentrated in the water
during the test.
D-1.3 Contniners, rontailling distilled water, or
\+.iiIcr of cquivaltnt purity quipput with a I~~C;IIIS 01 D-3.1.2 In general, place each set of three test speci-
hciiting awl capatllc 01’ king coaltollcd a1 tlic. mens in a separate container (D-1.3) with the spcci-
tcmpcratt1rc spccil‘ivd. mcns immcrscd completely in the watrr.
IS 13411: 1992
However, when several samples of the same composi- temperature. Take the specimens from the water and
tion have to be tested, it is permissible to place several remove all surface water with a clean, dry cloth, or
sets of test specimens in the same container. with filter paper. Re-weigh the specimens to the near-
est 1 mg within 1 minute of taking them from the water
In no case shall any significant area of the surface of a (mass mJ.
test specimen come into contact with the surface of
other test specimens, or with the walls of the container. D-3.5 Method 4

D-3.1.3 The times for immersion in the water are D-3.5.1 If it is desired to allow for the presence of
stated in D-3.2 and D-3.4. However, larger times ,water-soluble matter dry the test specimens again for
may be used by agreement between the interested 24 2 1 h in water oven, controlled at 50 ? 2OC, after
parties. In such cases the following precautions shall completion of Method 3 (D-3.4). Allow the specimens
be taken: to cool to ambient temperature in the desiccator and
re-weigh to the nearest 1 mg (mass m$.
- if testing in water at 27OC agitate the water at
least once daily, for example, by rotating the D-4 EXPRESSION OF RESULTS
containers.
D-4.1 For Methods 1 and 3, calculate for each test
- if testing in boiling water, add boiling water specimen the mass in milligrams, of water absorbed,
from time to time, as required to maintain the
according to the formula,
volume.

m2 - ml
D-3.2 Method 1
where
D-3.2.1 Dry three specimens for 24 t 1 h in the oven
controlled at 50 f 2OC, allow to cool to ambient ml is the mass, in milligrams, of the test specimrn
temperature in the desiccator and weigh each speci- before immersiop; ?nd
men to the nearest 1 mg (mass ml). Then place the “2
is the mass, in mllhgrams, of the test specimen
specimens in a container containing distilled water, after immersion.
controlled at 27 2 2OC.
D-4.2 For Methods 2 and 4, calculate for each test
D-3.2.2 After immersion for 24 + 1 h, take the speci- specimen the mass, in milligrams, of water absorbed,
mens fromthe waterand remove all surface waterwith according to the formula,
a clean, dry cloth or with filter paper. Rc-weigh the
m2-m 3
specimens to the nearest 1 mg within 1 minute of
taking them from the water (mass m,).
where
D-3.3 Method 2 m2 is as defined in D-4.1; and
9 is the mass, in milligrams, of the test specimen
D-3.3.1 If it is desired to allow for the presence of after immersion and drying.
water-soluble matter, dry the test specimens again for
24 r 1 h in the oven, controlled at 50 r 2OC, after D-4.3 For all four methods, express the results as the
completion of Method 1 (D-3.2). arithmetic mean of the three values obtained.

D-3.3.2 Allow the specimens to cool to ambient tem- D-4.4 Calculate for each test specimen the water ab-
perature in the desiccator and reweigh to the nearest 1 sorption as a percentage by mass of the initial mass, by
mg (mass m,). the following formula, as appropriate:

D-3.4 Method 3 m2 - m m2 - m
‘- x 100 or 3 x100
D-3.4.1 Dry three test specimens for 24 2 1 h in the
ml ml
oven, controlled at 50 2 2OC, allow to cool to ambient NOTE - If it is required to express the water absorption as a
temperature in the desiccator and weigh each speci- percentage of the mass of the test specimen after drying, use the
men to the nearest 1 mg (mass m,). Place the specimens formula:
in a container containing boiling distilled water.
m, - 5 x loo
D-3.4.2 After immersion for 30 2 1 min, take the 5
specimens from the boiling water and allow them to
cool for 15 -C 1 min in distilled water at ambient where m,. m, and m, are as defined in D-41 and D-42.
IS 13411: 1992

ANNEX E
[Table 2, SZ No. (iii) ]
DETERMINATION OF IZOD IMPACT STRENGTH
[ Adapted from IS0 180 : 1982 ]

E-O PRINCIPLE E-2.1.2 The machine shall have the characteristics


shown in Table 5. These characteristics shall be
The test specimen, supported as a vertical cantilever periodically checked.
beam, is broken by a single swing of a pendulum,
with the line of impact at a fixed distance from the Table 5 Characteristics of Pendulum Impact
specimen clamp and from the centre line of the Testing Machines
notch.
Impact Energy Velocity al MaXilttUttt Permissible
Impact Permlsslble Error After
For determination of the Izod impact strength of Frictional Loss correclioll
notched specimens, the pendulum strikes the face
containing the notch. For determination of the Izod J m/s o/o J
impact strength of reversed notch specimen, the pen- 1.0 3.5 (2 10 percent) 2 0.01
dulum strikes the face opposite to that containing the
notch. 2.75 3.5 (5 10 percent) 1 0.01

E-l DEFINITIONS 5.5 3.5 (2 10 percent) 0.5 0.02

11.0 3.5 (2 10 percent) 0.5 0.05


E-l.1 Izod Impact Strength of Notched Specimens
22.0 3.5 (2 10 percent) 0.5 0.10
The impact energy absorbed is breaking a notched
specimen, referred to the original cross-sectional area
of the specimen at the notch. E-2.1.3 The machine shall be securely fixed to a
foundation having a mass of at least 40 times that of the
It is expressed in kilojoules per square’meter (KJ/m2).
heaviest pendulum in use. It shall be adjusted so that
E-l.2 Izod Impact Strength of Reversed Notch the orientation of the striker and vice are as specified
in E-2.1.4 and E-2.1.6.
Specimens
E-2.1.4 The striking edge of the pendulum shall be
The impact energy absorbed in breaking a reversed
of hardened steel and shall have a cylindrical surface
notch specimen, referred to the original cross-sec-
having a radius of curvature of 0.8 2 0.2 mm, with its
tional area of the specimen at the notch.
axis horizontal and perpendicular to the plane of
motion of the pendulum. It shall be aligned so that it
It is expressed in kilojoules per square meter (KJ/m2).
makes contact across the full width of rectangular
NOTE -The reversed notch test gives an indication of the izod
test specimens. The line of contact shall be within ? 2”
impact strength of unnotchcd specimens. of perpendicular to the longitudinal axis of the test
spccimcn.
E-l.3 Relative Impact Strength
K-2.1.5 The distance between the axis of rotation and
The ratioofthe impact strengths of notched to reversed the centre of percussion of the pendulum shall be
notch specimens with the same notch base radius, or of within t 1 percent of the distance from the axis of
notched specimens with different nolch radii, for lest rotation to the point ofcontact ofthestrikingedge with
specimens of the same type. the test specimen.
E-2 APPARATIJS E-2.1.6 The lest spccimrn support shall comprise a
vice consisling of a fixed and movable jaw. The
E-2.1 Testing Machine (,lamping surfaces of the jaws shall be parallel lo
u Ilhllh 0.025 mtn. The vice shall be so arranged that it
E-2.1.1 It shall be of the pendulum lypc and shall h htrlds Ihr test specimen vertically in rcsllect to its
of rigid construction. It shall be capable of measuring long axis and at right angles IO the lop plane of the
the impact energy expressed in breaking a test speci- vice (see Fig. 2). The top edges of the vice jaws shall
men, the value of which shall be taken as equal to the have radii of 0.2 + 0.1 mm. Means shall bc provided
difference between the initial potential energy in the lo ensure that when the test sprcimen i\ clamped in
pendulum and the energy remaining in the pcndulunl Ibr vice, thr top plane of thr vice is within 0.2 mm of
after breaking the test specimen. The energy scale Ihe plane bisecting rhr angle of the notch.
shall be accordingly corrected for friction and air
resistance losses and scale errors. The vice shall be positioned so that the test spccimcn
NOW - Falling weight gyp machines may bc utrd II they can is crntml, to within 2 0.5 mm, to the striking edge atld
be shown IO give the same rrsula AS pendulum ~ypc mwhines so I hat the centre of the striking edge is 22.0 2 0.2 mm

11
IS 13411: 1992
above the top plane of the vice (see Fig. 2). The E-3.1.2 Specimens taken from sheet thicker than
vice shall be designed to prevent the clamped portion 12.7 mm shall be milled uniformly on both surfaces to
ofthe test specimen from moving during the clamping achieve a thickness 12.7 2 0.2 mm.
of testing operations.
When testing sheet materials in the edgewise direc-
E-2.2 Micrometers and Gauges tion, test specimens shall be cut so that the thickness of
the sheet is dimension x (see Fig. 3). When testing
Micrometers and gauges suitable for measuring the sheet materials in the flatwise direction, the test speci-
essential dimensions of test specimens to an accuracy mens shall be cyt so that the thickness of the sheet is
of 0.02 mm are required. dimension y (see Fig. 3 to 6).
E-3 TEST SPECIMENS E-3.1.3 Notches shall always be cut so that the di-
mensionx is the length of the notch (see Fig. 3 and 4).
E-3.1 Dimensions and Notches
E-3.2 Procedure
E-3.1.1 Four types of test specimens with two differ-
ent types of notch may be used as specified in Tables E-3.2.1 A panel shall be prepared from the
6 and 7, and shown in Fig. 3 and 4. compound in accordance with 7.1 and specimen shall
be machined therefrom.
The preferred type of test specimen is type 1, and
the preferred, type of notch is type A. However, the E-3.3 Notched Specimens
type or specimen and the type of notch will be indi-
cated in the specification, if any, for the material E-3.3.1 Notches shall be machined on unnotched
being tested. Test specimen types 2, 3 and 4 differ specimens prepared in accordance with E-3.2.
only in width (dimensionx). The type of notch will also Notching shall be carried out on a milling machine or
depend on the information required from the test. lalhc, with a cutter which may be of the single-tooth
NOTE - Notch type A has been adopted as the preferred type for or multi-tooth variety. The single tooth cutter is pre-
the determination of Izod impact strength. Carrying out tests ferred because it is more readily ground to the desired
with both notch typesAand B(that is, at hvo well-defined notch
contour. The cutting edge shall be carefully ground
base radii) overa range of temperatures may provide valuable in-
formation on the variation of notch sensitivity of the material and honed to ensure sharpness and freedom from
with temperature (ductile/brittle transitions). nicks and burrs. Tools with no rake and a work relief
angle nf 15 to 20” have been found to be satisfactory.
Table 6 Specimen Types and Dimensions
The profile of the cutting tool (teeth) shall be such as
to produce in the specimen, at right angles to its prin-
Specimen Length, I Dimension, y Yreferred Value
of Dimension .X ripal axis, a notch of the contour and depth shown in
Type
Fig. 3 and 4.
(1) (2) (3) (4)
1 x0.0 + 2 10.0 + 0.2 4.0 f 0.2 E-3.3.2 In the case of single-tooth cutters, the con-
2 63.5 2 L 12.7 r 0.2 12.7 + 0.5 tour of the tip of the cutting tool may bc checked
3 63.5 2 2 12.7 ir 0.2 6.4 ? 0.3 instead of the contour of the notch in the spccimcn, il
4 63.5 r 2 12.7 + 0.2 3.2 c 0.2 it can be shown that the two correspond or lhal a
definitive relationship exists between them for the
specific type of material being notched. There is some
Table 7 Specimen Types, Notch Types and cvidencc that notches cut by the same cutter in mate-
Notch Dimensions rials of widely differing physical properties may
differ in contour.
Specimen Type Notch Type Notch Dimensions, mm
The radius of Ihe notch base shall be 0.25 2 0.05 nm
(1) (2) (3) for type A notches (See Fig. 3) and 1.OO+ 0.05 mm for
1 A y, = 8.0 5 0.1 type B notches (see Fig. 4).
1 B yr = 8.0 r 0.1
1 Reversed ~~-8.0 ? 0.1
E-3.3.3 A linear speed of Ihc tip of the cutting tool 01‘
about 90 to 1X5 m/min, and feed rates in the range from
2 A y, =I02 c 0.1 10 to 130 mm/min, have been found to be satisfactory
2 R yr z10.2 ? 0.1 for some materials. When unfamiliar materials are to
2 Reversed _VI =10.2 z 0.1 be notched, it may bc necessary to detcrminc the rffrci
of variation of the cutting speed.
3 A 4’, =10.2 5 0.1
3 B y, =10.2 5 0.1 E-3.3.4 After each 500 notches, or more often if hard
3 Reversed y, =10.2 * 0.1 abrasive materials are notched, the cutter shall hr
inspected for sharpness, freedom from nicks, tip
4 A y, z10.2 + 0.1
radius and contour. If the radius and contour do not
4 Lt yt =1x! + 0.1
fall within their specified limits, Ihe cutler shall bc
4 Reversed yk =lU.L % 0.1
rcplacrd by a nrwly sharpened and honed enc.

12
IS 13411: 1992
A microscope with a camera lucida attachment (X 60 E-4.2 Adjust the pointer on the energy scale so that
magnification) is suitable for checking the notch base. it touches the driving pin when the pendulum is in
Relatively close tolerances have to be imposed on -the starting position. Carry out a blank test (that is,
the contour and the radius of the notch for most without a specimen in place) and ensure that the total
materials, because these factors largely determine the frictional losses do not exceed the values given in
degree of stress concentration at the base of the notch Table 5.
during the test. The maintenance of a sharp,
clean-edged cutting tool isparticularly important since E-4.3 Measure the dimensionx of the test specimen,
minor defects at the base of the notch cati cause to the nearest 0.02 mm. Carefully measure the
large deviations in the test results. Particular attention dimension y using, for example, a micrometer fitted
shall be given to the accuracy of the dimension y, with an anvi *Fof width 2 to 3 mm and of suitable profile
(see Table 7). to fit the shape of the notch. Carry out two measure-
ments, one at each end of the notch, and calculate the
E-3.3.5 Abradants shall not be used in preparing the mean value.
notch.
E-4.4 Lift and arrest the pendulum, and adjust the
E-3.3.6 Specimens with moulded-in notches may be pointer in accordance withE-4.2. Place the specimen
used if specified in the specification for the material in the vice and clamp it in accordance with E-2.1.6
being tested. as shown in Fig. 2. For the determination of notched
Izod impact strength, notch shall be positioned on
NOTE - Specimens with moulded-in notches do not give the the side that is to be struck by the striking edge of the
same resultsasspecimenswith machinednotchesandallowance
pendulum (see Fig. 2). For the determination of
should be made for this difference in interpreting the results.
Specimens with machined notches are generally preferred reversed notch Izod impact strength, specimens shall
because skin effects and/or localized anisotropy are minimized. be positioned so that the notch is on the opposite
side to that to be struck by the striking edge of the
E-3.4 Number pendulum.
E-4.5 Carefully release the pendulum. Read from the
E-3.4.1 Unless otherwise, specified in the specifica-
scale the impact energy absorbed by the specimen,
tion for the material being tested, a minimum of ten
and apply such corrections for frictional losses, etc, as
specimens shall be tested.
may be necessary.
E-3.4.2 Certain types of sheet materials may show E-4.6 For calculation of test results, only completely
different impac! properties according to direction in broken specimens shall be taken into consideration.
the plane of the sbeet. ln such cases, it is customary Certain materials may, however, exhibit hinged
to cut two groups of test specimens with their major breaks where the specimen remains joined by a very
axes respectively parallel and perpendicular to the thin moulding skin; such breaks are acceptable.
direction of some feature of the sheet which is either
visible or inferred from a knowledge of the method of E-5 CALCULATION AND EXPRESSION OF
its manufacture. RESIJl ,TS

E-3.4.3 Laminated sheet materials are normally tested E-S.1 The lzod impact strength of notched specimens
in the edgewise direction. However, sheets of nomi- a, in kilojoules per square mctre, is given by the
nal thickness 12.7 mm or greater may, if specified, be formula:
tested in both the edgewise and flatwise directions
(see E-3.4.2 and Fig. S and 6).
uk
= - A, x II-J-’
x . Yk
E-3.5 Conditioning
where
E-3.5.1 Unless otherwise, specified in the spccifica- A, is the impact energy, in joules, absorbed by the
tion for the material being tested, the specimens test specimen;
shall be preconditioned and tested in accordance with X is the dimension x, in millimetrrs, of the test
IS 196 : 1966. specimen; and
E-4 PROCEDLJRE Yk is the dimension yk, in millimetres, of the test
specimen.
E-4.1 Check that the pendulum machine is of the E-5.2 The Izod impact strength of reversed notch
correct energy range and that it has the specified specinlcns, u, in kilojoules per square metre, is givcu
striking velocity (see Table 5). by the formula:

The selected peridulum shall consume at least 10 A


percent, but not more than X0 percent, of its stored
CL, = - x IO3
energy in breaking the test specimen. If’ more than x . Y,
one of the pendulum5 described in Table S meet these whcrc
requiremeuts, the pendulum having the highest energy A is the impact energy, in joules, ahsorhcd by the
shall be used. test specimen;

13
IS 13411: 1992
X is the dimension x in millimetres, of the test deviation and the coefficient of variation of the ten
specimen; and lTSUlt.S.

E-S.4 If required, calculate the relative impact strength


yk is the dimension y, in millimetres, of the test for any two notch types as defined in E-1.3, and
specimen. express the result as a percent.

E-53 Calculate the arithmatic mean, rhe standard E-5.5 Report all calculated values to two significant
figures.

ANNEX F
[Table 1, Sl No. (iv) ]

DETERMINATION OF FLEXURAL STRENGTH


[ Adapted frvm IS0 178 : 1975 ]

F-O GENERAL not exrecd + 1 percent and for indicated deflection


does not exceed 2 2 percent.
This method applies only to a simple, freely sup-
ported beam, loaded at mid-span (three-point loading NOTE - It is recommended that a machine lx used which has
less than2mm movcmentofthe weighingmechanism forthe full
test). scale load.
NOTE - Four-point loading lest, a method in which the load is
applied by two loading noses. allows measurement of a pure
flexural stress in the middle part of he test piece. The compres-
The radius r, of the loading nose and the radius r2 of
sive stresses due to the two central noses are much lower in the supports shall be as follows:
comparison with the stresses induced under the one central
loading nose of the three-point test. r, : 5 2 0.1 mm;
rz : 0.5 + 0.2 mm for thickness of the test piece
F-l DEFINITION
up to and including 3 mm; and
F-l.1 Deflection 2 + 0.2 mm for thickness of the test piece over
3 mm (see Fig. 8 ).
The distance over which the top or bottom surface of
the test piece at mid-span has deviated during flexural The span shall be adjustable.
from its original position.
F-3 TEST PIECES
F-l.2 Flexural Stress at a Given Time of the Test
F-3.1 Prepare bars of rectangular cross-section as
The maximum outer fibre stress of the material in the
section of the test piece at mid-span. It is calculated described in 7.
according to the relationship given in F-5.1.
F-3.1.1 Standard Test Pieces
F-l.3 Flexural Stress at the Conventional
The standard dimemions in millimetres shall be:
Deflection
The flexural stress at a deflection equal to 1.5 times the length I = 80 or more
thickness of the test piece. width 6 = 10 2 0.5
thickness h = 4 + 0.2
F-l.4 Flexural Stress at Maximum Load
The flexural stress developed when the load reaches F-3.1.2 Olher Test Pieces
the first maximum.
When it is not possible or desirable IO use the
standard test piece, the following rules shall bc
F-l.5 Flexural Stress at Rupture
observed, except as noted below:
The flexural stress developed at the moment of
rupture. a>The length and thickness of the test piece shall
be in the same ratio as in the standard test
F-2 APPARATI JS piece, that is:
I, Min = 20 II
F-2.1 Standard Testing Machine
Properly constructed and calibrated, which can be b) The width of the test piece may bc any v;liuc
operated at an approximately co~tsta~~l rate, V, 01 between IO and 25 mm rxcept for nc+tcrials
relative movement of the loading IIOSC and the sup- with very coarse fillers for which thr width
ports, and in which the crrnr for indicated loads does shall be 20 to 50 mm.

14
IS 13411: 1992
NOTE - The preparation and dimensions of the test piece may Measure the length of the span to within 0.5
bedefined by the specification for the material. Alternatively, the
percent.
values of width given in the table below may be usal:
NOTE- For very thick and unidirectional fibre-reinforces test
Fibre-Reinforced Plastic.s pieces it may be necessary to use a distance between sup-
. ports calculated on a higher ratio of L/h lo avoid delamination in
All dimensions in millimetres. shear.
Nominal Thickness Width For very thin test pieces, it may be necessary to use a distance
h b between supports calculated on a lower value of L/h IO enable
measurements to be made within the load capacity of the testing
l<b* 10 15 machine.
\
lO<hb 20 30
r 0.5 F-4.3 For testing to a specification, V(relative rate of
20 < h e 35 50 movement of the loading nose and supports) shall be as
i
35 c h ,< 50 80 /
required in the specification for the material.

NOTE 1 - If desired, V may be calculated as follows:


When very coarse textile glass Iibre roving is used as
the reinforcement, it may be necessary to increase the SrL2
width of the test pieces. V= -
6h

F-3.2 Aaisotropic Materials where

F-3.2.1 In the case of anisotropic materials, the test V is the relative rate of movement of the loading nose and
pieces shall be chosen so that the flexural stress in supports in millimetrea per minute:
the test procedure will be applied in the same direc- Sr is the strairl rate, per minute, 0.01 or as required by the
tion as that to which products (moulded articles, material specification;
sheets, tubes, etc) similar to those from which the test
pieces are taken, will be subjected in service. The L is the span length in millimetres; and
relationship of the test piece chosen to the application h is the thickness of the test piece in millinxztres.
will determine the possibility or impossibility of using
standard test pieces and, in the latter case, will NOTE 2 - When ther? is no specification for the fibre-rein-
govern the choice of the dimensions of the test forced material to be tested. one or the otherof the two following
pieces in accordance with F-3.2. It should be noted methods can be used:
that the position or orientation and the dimensions of
Method A : for qualification testing of the material
the test pieces sometimes have a very significant
when L/h = 16 + 1
influence on the test results. This is particularly true of V(mm/min) = h/2 (mm)
laminates (see Fig. 7 ).
Method B : for routine and screening tests
F-3.2.2 When the material shows a significant V = 10 mm/min
difference in flexural properties in two principal
directions, it is to be tested in these two directions. If, F-4.4 Load the test piece as a simple beam at mid-
&cause ofthe application, this material is subjecied to span without impact (see Fig. 8).
stress at some specific orientation to the principal
direction, it is desirable to test the material in that
F-4.5 If it is desired to measure the modulus of
orientation.
elasticity, read the load and the deflection values
simultaneously sufficiently frequently so that a
F-3.3 Number of Test Pieces
smooth load-deflection curve may be plotted.
W-3.3.1 At least fivr test pieces shall be tested.
F-4.6 For test pieces that rupture bcforc, or al, the
F-3.3.2 The results from test pieces that break out- moment of reaching Ihe cmvenlioual dcflcction
side the central one-third of the span length shall be (see F-1.3), record the load and dellcction at
discarded and new test pieces shall be tested in their rupture.
place.

F-3.4 Conditioning of Test Pieces


The test pieces shall be conditioned as per 7.2.

F-4.1 Carry out the test in (one of the) standard


atmosphere specified in IS 196 : 1966.
F-4.2 Measure the width, 6, of the lest piece lo the F-4.8 For trh~ picccs Ihal show IIMX~IIWI~ load
nearest 0.1 mm and the thickness, Ir, to the ncarcst 0.02 before lhc corivcnlioual deflectiorl i<. rcachcd,
mm. Adjust Ihe length of thr spau, L, IO : record Ihe n~axir~~u~~l load and Ihe colnt’hlxludiup
L = 1s h to 17 I1 dellection.
IS 13411: 1992
F-5 EXPRESSION OF RESULTS F-S.2 To calculate the apparent modulus of elasticity,
E,, in megapascals, a load-deflection curve is plotted
F-S.1 The flexural stress, a, at a load F is calculated, using the data collected. The modulus of elasticity is
in megapascals from the formula: determined from the initial linear portion of the load-
deflect curve by using at least five values of the
M
a, = -- deflection and the load for the test piece, E,, is given
W by the following formula:
where
L3 F
M is the flexural moment at load F, given by the E,=-x-
4 bh3 Y
formula:
where
FL
M=- E, is the modulus of elasticity;
4 L is the span length;
in which b is the width of the test piece;
h is the thickness of the test piece;
F is the applied load, in meganewtons; F is the load at a chosen point on the initial linrar
L is the span length in metres; and portion of the load-deflection curve; and
W is the section modulus, in cubic metres.
Y is the deflection corresponding to load F.
For a rectangular section:
If L, b, h and y are in millimetre, and F is iu newton,
bh2 then E, is in N/mm2 which is numerically equal to MPa
WC----- and if L, b, h, and Y are in millimetrcs but F is in
6
kilogram-force, then E, is in kgf/mm*.
and
F-S.3 The calculated flexural stress is that which
3 FL
Of = occurs at the surfaces of the test piece, assuming that
2 bh2 the neutral axis is the middle of the thickness.
NOTES
During a flexural test, three different types of breaks
can occur:
1 If M is expressed in newton millimetres and W in cubic
millimetres,a,is obtained in N/mm’, numerically equal to MPa.
a) rupture due to tensile stresses;
b) rupture due to compression stresses; and
IfMisexpressed in kilogram-force millimetres.and Wisincubic
millimetres, cr, is obtained in kgf/mm’. c) rupture due to shear stress.
The type (s) of break which occur(s) must br indicated
2 For a more accurate calculation of the flexural stress which
takes into account the horizontal component of the flexural for each test piece.
moment at deflection d, the following equation may be used:
If the types of rupture observed in testing a group 01
3FL 4 test pieces are different, then the values obtained for
C?,= - It
2 bh2 C L’ 1 flexural stresses are statistically in homogeneous. In
such a case it is necessary to carry out a critical study
where, d is the deflection at mid-span in millimetres. of all the results and to examine with great care the
arithmetic mean values and stalislical deviations.
The other terms are as previously defined.
IS 13411: 1992

ANNEX G
[ (Table 2, Sl No. (ix) ]

DETERMINATION OF POWER ARC RESISTANCE


( APapted from ASTM D 495-84 )

G-O. GENERAL G-l SIGNIFICANCE AND USE

G-0.1 This test method is intended to differentiate, in G-l.1 The high voltage, low-current type of arc
a preliminary fashion, among Similar materials with resistance test is intended to simulate only approxi-
respect to their resistance to the action of a high- mately such service conditions as exist in alternating
voltage, low-current arc close to the surface of insula- current circuits operating at high voltage, but at
tion, intending to form a conducting path therein or in currents limited to unit and tens of milliamperes.
causing the material to become conducting due to the
localized thermal and chemical decomposition and G-l.2 In order to distinguish more easily among
erosion. materials which have low arc resistance, the early
stages of this test method are mild, and the later stages
G-O.2 The usefulness of this test method is very sev- are successively more severe. The arc occurs
erly limited by many restrictions. Generally, this test intermittently between two electrodes resting on
method should not be used in material specifications. the surface of the specimen, in regular or inverted
Wheneverpossible, alternative test methods should be orientation. The severity is increased in the early
used, and their development is encouraged. stages by successively decreasing to zely) the
interval between flashes of uniform duration, and in
G-O.3 This test method will not, in general, permit later stages by increasing the current.
conclusions to be drawn concerning the relative arc
resistance rankings of materials which may be sub- G-l.3 Four general types of failure have been
jected to other types of arcs, for example, high voltage observed.
at high currents, and low voltage at low or high
currents (promoted by surges or by conducting G-1.3.1 Many inorganic dielectrics become incan-
contaminates ). descent, whereupon they are capable of conducting
the current. Upon cooling, however, they return lo
G-O.4 The test method is intended, because of its their earlier insulating condition.
convenience and the short time required for testing,
for preliminary screening of material, for detecting G-1.3.2 Some organic compounds burst into tlame
the effects of changes in formulation, and for quality without the formation of a visible conducting path in
control testing after correlation has been cstab- the substance.
lished with other types of simulated service arc tests
and field experience. Because this test method is G-1.3.3 Others are seen to fail by ‘tracking’, that is, a
usually conducted under clean and dry laboratory thin wiry line is formed between the electrodes.
conditions rarely encountered in practice, the predic-
tion of a material’s relative performance in typical G-1.3.4 The fourth type occurs by carbonization of
applications and in varying ‘clean to dirty’ environ- the surface until sufficient carbon is present to carry
ments may be substantialy altered. Caution is urged the current.
against drawing strong conclusions without cor-
G-l.4 Materials often fail within the first few
roborating support of simulated service tests and
seconds after a change in the severity stage. When
field testing. Rather, this test method is useful for
comparing the arc resistance of materials, much more
preliminary evaluation of changes in structure and
weight should be given to a few seconds that
composition without the complicating inlluence of
overlap two stages than to the same elapsed time
environmental conditions, especially dirt and
withina stage. Thus, there is a much greater difference
moisture.
in arc resistance between 178 to 182 s thau between
NOTE - F3y changing some of the circuit condition dcscrihed 174 and 178 s.
herein it has been foundpossihlc to rearrange markedly the order
of arc resistance of a group of organic insulating materials G-2 DFFINITIONS
consisting of vulcanized fibre and of moulded phcnolic and
amino plastics, some containing organic, and some inorganic
filler.
G-2.1 Arc Resistance
The total elapsed time (seconds) of operation of the
G-0.5 This test method is not applicable to materia!s test until failure occurs.
that do not produce conductive paths under the action
of au c,lectric arc, or that melt or form fluid residues G-2.2 Failure
which float conductive residues OUI of the active test
area thereby preventing formation of a conductive For materials for which this test method has mosl
path. mtaningand significance, the end point, or ‘failure’ is

17
IS 13411: 1992
usually quite definite in that a conducting path is of arc resistance greater than 180 s, the use of the
formed across the dielectric, the arc disappears into tungsten rod electrodes is recommended because
the material, and a noticeable change in sound the comers of the stainless steel strip electrodes
takes place. For some materials, bowever, tbe descrip- erode appreciably under such conditions. Results
tion of failure is more difficult. In these cases, failure obtained with the use of the tungsten rod electrode
is described as follows. system may be different from those obtained with tbe
use of the stainless steel strip electrode system.
G-2.2.1 The trend towards failure increases over a
fairly broad interval of time before all parts of the arc G-4 APPARATUS
have disappeared. In this instance the end point, or
‘failure’, is considered to have been reached only G-4.1 The apparatus (see Fig. 9 for electrical circuit)
when all parts of the surface between the electrodes is closely specified to maximize data reproducibility
are carrying the current; that is, no portion is appar- among different test sets. The arc obtained will be
ent as an arc. relatively quiet, rather tban the crackly blue spark
characteristic of a condenser discharge. Primary
NOTE- In restingsomematerials, a persislenl scintillation will
be observed close to the electrodes after a tracking path obvi-
voltage control is made by a variable transformer
ously has been completed. 7he persislence of lhis remaining rather than by a variable inductance because of its
scintillation is not Lo be counted as part of the arc r&stance proved deleterious affect on the perfomutnce of the
time. arc.

G-2.2.2 Burning of the material obscures the arc. It G-4.1.1 Transformer T,


may be preferable in such cases to report simply that
failure occurred by burning. A self-regulating transformer (non-power factor cor-
rected) with a rated primary potential of 115 Vat
G-2.2.3 In successive arc intervals the dielectric con- 60 Hz ac, a rated secondary potential (on open circuit)
ducts the current only in the later part of the ‘on’ of 15 000 V, and a rated secondary current (on short
time. The first such interval should be designated as circuit) of 0.060 A.
failure.
NOTE - The rated primary potential of transformer TVof 115 V,
60 Hz ac could be supplied from a suitable main transformer
G-2.2.4 When materials behave as described rated at 240 V/115 V 50 Hz to suit IndIn conditions.
in G-05, simply report by the type- behaviour and the
statement ‘Test not applicable for this material’. G-4.1.2 Variable Autotransformer, T,
G2.3 Orientation An autotransformer rated at 7 A or more, and nomi-
nally adjustable up to 135 V.
In normal orientation, the electrodes are placed on
top of the specimen. In inverted orientation, the elec-
G-4.1.3 Voltmeter, VI
trodes are placed on the underside of the specimen in
order to achieve closer contact of the arc to the speci- An ac voltmeter, readable to 1 V in the range 90 to 130
men. The inverted configuration is a more severe test V, is permanently connected across the output of the
and in many tests produces less data dispersion. autotransformer to indicate the voltage supplies to the
primary circuit.
G-3 INTERFERENCES
NOTE - A constant primary voltage supply is recommended.
G-3.1 It has been found that changes in the timing of Commercially available line voltage stabilizers which do not
distort the voltage waveform are suitable.
the intern&tent arc, and in the current, as well as other
circuit changes affecting the nature of the discharge,
does not only affect the duration of a test of most G-4.1.4 Milliammeter, A
samples in a group of dissimilar materials, but can An ac milliammeter capable of reading from 10 to 40
draslically alter their positions in order of rank. It is mA with an error of not over + 5 percent. Before use,
therefore, obvious that data obtained by this test to make certain of its readings, this meter should be
method, and the arbitrary conditions of test that have calibrated in a test circuit containing no arc gap. Since
been assigned, should not be employed to infer that this milliammeter is used only when setting up or
the materials examined occupy an unchanging quality making changes in the circuit, it may be shorted out by
relationship to each other, regardless of conditions of a by-pass switches when not in use.
anticipated use.
NOTE - Although provision has been made for rhe suppression
of radio-frequency components of cumnl in the arc. it may be
G-3.2 This test method describes two electrode desirable Io check for their presence when the apparatus is first
systems : stainless steel strip and tungsten rod. When construcied. This is done by use of B suitable Ihcrmocouple-type
testing materials with poor to moderate arc resistance r-f milliammet~r temporarily inserted in sprier with the milliam
(up to 180 s), the stainless strip electrodes shall be meter.

used in order to decrease the variability often


associated with the use of the rod electrodes. It is G-4.1.5 Current Control Resistors, R,, , R,, , R,,, RdO
permissible to make: additional tests with rod Four rcsisturs are required in series with the primary
electrodes, so as to provide a basis forcomparison with of T, but in parallel with each other. These resistors
other data obtained with such electrodes. For values must 1~ adjustable, to some cxtcnl, to permit exact

18
IS 13411: 1992

settings of the currents during calibrationR,,is always primary circuit and providing the intermittent arc
in the circuit to provide a 10 mAcurrent. Its value is ap- cycles listed in Table 8.
proximately 60, with a current rating of at least l’/,A.
Closing switch S,, to add R,, in parallel with R O,will G-4.1.14 High Voltage Switch, S,
provide a 20 mA arc current. R is about 50 h with
A single-pole, single-throw switch insulated for
a current rating of at least 13/ x. Similarly, R and
15 000 V ac. This switch must be isolated from the
R,, have values of about 30 and 15 respectively~“with
operator by a suitable enclosure through which
associated current ratings of 2 and 5 A. These resis-
projects an insulating handle of sufficient length to
tors, when switched in, provide arc current of 30 mA
ensure operator safety.
and 40 nlA respectively.
G-4.1.15 Wiring
G-4.1.6 Suppressing Resistors, RI
All wiring in the arc circuit must be of ignition wire
Rated at 15 000 S2 and at least 24 W. This resistor,
rated at 15 kV or higher, and must be so disposed that
along with the inductors in G-4.1.7, is used to
it and any circuit components are not readily
suppress parasitic high frequency in the arc circuit.
assembled when energized.
G-4.1.7 Air Core Inductors
G-4.1.16 SharpeningJigfor Tungsten RodElectrodes
Inductance totallingfrom 1.2 to 1.5 His obtained from
A steel jug for securing the electrodes during sharp-
about 8 coils of No. 30 cotton or enamel coated
ening to ensure finishing the pointed tips to the proper
covered wired. A single coil of this inductance is not
geometry (see Fig. 10).
satisfactory. Each coil consists of 3 000 to 5 000 turns
of wire wound or insulating non-metallic cores of
G-4.1.17 Stainless Steel Strip Electrodes
about (l/L? inch) 12.7 mm diameter and (S/8 inches)
15.9 mm itaide length. Cut (0.006 inches) 0.15 mm thick stainless steel into
(112 by 1 inch) 12.7 by 25.4 mmstrips. (The edges must
G-4.1.8 Interruptor, I be free of burrs.) Bend each strip slightly in the
middle of the lon dimension to form an angle of
This motor-driven device is used to give the re-
approximately 16 $ .
quired cycles for the three lower steps of the test by
opening and closing the primary circuit according to
G-4.1.18 Tungsten Rod Electrodes (see G-3.2 for
the schedule in Table 8, with an accuracy of ?: l/120 s
restrictions)
or better. The interruptor can be a synchronous motor
driving three appropriate sets of cams which actuate Make the electrodes from (3/32 inches) 2.4 mm
the contactor switches. diameter tungsten rod (tungsten welding rod has been
found suitable) which is free of cracks, pits or rough
G-4.1.9 Timer, TT spots, Use rods about (13/, inches) 45 mm long in the
electrode assembly, or use shorter rod lengths
A stop watch or electric interval timer operating at
fastened into a square shank (see Fig. 11) by swaging,
11.5 V ac, accurate to 1 s.
brazing or silver soldering, leaving an exposed
length of about (3/4 inches) 19 mm. The shank ensures
G-4.1.10 Indicator Lamp, IL
correct orientation of the electrode point after shar-
A6W,115Vlan1pwitha2oiK)52resistor,R ,inseries. pening (see G=7.2.2), although correct orientation of
This lamp indicates the interrupting cycles being used the simple rod electrode may be obtained by
and permits the operator to start the first cycle of each adjustment of the rod in the electrode assembly. In
test in a uniform manner by closing S,,, just after the either type of rod electrode, grind the end of the rod at
lamp is extinguished. a 300 angle to the axis (see Fig. 11) to achieve a flat
elliptical face. Exercise care in grinding to prevent
G-4.1.11 Control Switches cracking or chipping.
Toggle switches are convenient. All may be of the G-4.1.1 9 Electrode Assemblies
size rated at 3 A and 110 to 125 V ac, except S,, and
S,,, which require 10 A ratings. These assemblies provide a means of holding the
electrodes and specimens and of applying the arc to
G-4.1.12 Safer>,Interlocking Contactor, CI the top surface of the specimen. Construct each
assembly, whether for stainless steel stripclectrodes or
Rated at 10 A and 110 to 125 V ac, this interlocking for tungsten rod electrodes, so that the lop surface of
contactor is installed so that raising the draft shield each specimen is at the same level height. Provide
around the electrode assctl~hly will open the contac- ample air space below the specimen, especially in the
tor and thus remove high voltage from the electrodes. region directly below the test area. Adjust each
electrode so that it rests independently with a force
G-4.1.13 Inlerrrrptor Contactors, C,,, , C,,, , C,,, of 50 2 5 g on the top of the spccimcn. Provide A
transparent shield around the assembly to protect the
Normally, open spring contactors, rated at l/A (or specimen from air drafts, and allow venting oi
better) and 125 V ac. These contactors are operated by combustion products in cases where sperimcns
the interrupted cams, thus closing and opening the give off toxic smoke or gases during the ~rst.

19
IS 13411: 1992
Protect the operator from inadvertant contact with It is essential that the test apparatus and all associated
the electrodes, and provide a clear view of the arc from equipment that may be electrically connected to it be
a position slightly above the plane of the specimen. properly designed and installed for safe operation.

Table 8 Sequence of 1-Min Current Steps G-5.2 Solidly ground all metal parts that any person
( Cluuses,G-4.1.8 and G-4.1.13 ) might come into contact with during the test.

current, mA Time Cycle* TotaI Time, s G-5.3 Thoroughly instruct all operators in the proper
SkP
way to conduct the test safely.
0) (2) (3) (4)

l/4 s on, l’/, s off 60


G-5.4 When making tests at high voltage with elec-
l/8 10 10
trodes, the energy released at breakdown may be
l/4 10 10 l/4 SO”, 314 s off 120 sufficient to result in fire, explosion, or rupture of
l/2 10 10 l/4 son, l/4 a off 180 the test chamber. Designof test equipment, test cham-
10 10 continuous 240 bers, and test specimens should be such as to minimize
the possibility of such occurrences, and to eliminate
20 20 continuous 300
the possibility of persona1 injury.
30 30 continuous 360
40 40 continuous 420 G-6 SPECIMEN$AND NIJMBER OF TESTS
l In the earlier steps an interrupted arc is used to obtain a 1~s
G-6.1 For standard comparison of materials, test at
severecondition than thecontinuousarc; acurrentofless than
least five specimens (0.125 2 0.010 inches) 3.17 + 0.25
10 mA produces an unsteady (flaring) arc.
mm in thickness. Make each test on a flat surface
of the specimen, with each lest area not closer than
G-4.1.19.1 Stainless steel strip electrode assembly
(l/4 inches) 6.4 mm to the specimen edge nor closer
(see Fig. 12 and 13)
than (l/2 inches) 12.7 mm to a previously tested area.
Place two stainless steel strip electrodes on the top of Test thin materials by first clamping them together
thespecimensurface with thecorners downand spaced tightly to form a specimen as close as possible to the
(0.250 + 0.003 inches) 6.35 2 0.08 mm apart, and at recommended thickness.
angles of 4S” to a line joining the corners. Either use
an electrode holder such as the one in Fig. 12 and 13, G-6.2 When testing moulded parts, apply the arc to a
or use the rod electrode assembly with the rods sepa- location deemed most significant. Make all compari-
rated and resting on the stainless steel strip electrodes. son tests of parts in similar locations.

G-4.1.19.2 Tungsten rod electrode assembly (see G-6.3 Dust, moisture, or finger ntarks can affect the
Fig. 11 and 14) time required to track. If affected, clean specimens or
parts with a cloth containing water or other suitable
Position the electrodes so that they lie in the same solvent before conditioning. Wipe such specimens
vertical plane and are both inclined 35O from the with a dry cloth immediately before testing.
horizontal (thus inclined 1100 between their axes).
Check to see that the minor axes of the elliptical tip NOTE - If the purpose of the test is IO ascertain the effect of
surfaces are horizontal, and space the tips (0.250 t contaolination, theseinstructionsmay bedisregarded. However,
0.003 inches) 6.35 2 0.08 mm apart. The proper orien- state the nature and quantity of contaminant present (if known)
tation will automatically be obtained if the following in the report.
factors are controlled:
G-7 CLEANING AND SHARPENING
a>Axis of tungsten rod is perpendicular to the EIXCTRODES
axis of the support rod,
G-7.1 Stainless Steel Electrodes
b) Support rods are gripped in the pivot in a
position such that the axis of each electrode is Use two new corners ol’ the stainless steel strip clew-
inclined at 35O when the support rods are trodes for each test. Replace electrodes after four tests.
horizontal, Other than inspecting the electrode corners to be
sure that they are free of burrs, no cleaning or
c) Electrodes are mounted in square shanks and
sharpening is required.
sharpened in a correctly made jig, and

4 The spacing between electrode tips is adjusted G-7.2 Tungsten Rod Electrodes
with the support rods in a horizontal position.
G-7.2.1 If excessive accumulations of products of
Ifelectrodesare not mounted insquareshanks,
decomposition occur, clean the rod elcctrr~des genlly
obtain proper orientation by adjusting and
with laboratory tissues. The application of a continu-
rotating the electrodes after they are inserted
ous 4U 11~4arc for approximately 1 min (wilhoul ;I
in the appropriate electrode assembly.
spccimcn in place) ofien proves Lo be the most cffcc-
tivc ccchniquc of cleaning the clcctrodcs.
G-5 SAFETY PRECAI.~IONS
(i-7.2.2 Sharpen the tungsten rod electrodes when
G-5.1 Lethal voltages may be present during this test. examination of Ihe tip edge shows that iI has been

20
IS 13411: 1992

rounded to a diameter of (0.030 inches) 0.08 mm, or ings in which the test will be run, prevent condensation
when burrs or rough edges are observable at 15 x on the specimens by warming the specimens in a dry
magnification. First, polish the rod surface by rotat- atmosphere.
ing it on its axis using successive grades of emery
paper (form No. 1 to 000) held between the fingers. NOTE - Warming the specimen in a 500 oven for about
30 minutes is suitable in most cases.
Then mount the electrode in the sharpening jig (see
Fig. 10) with its elliptical face flush with the surface of
G-10 PROCEDURE
the jig. Hold the surface against a rotating polishing
disk or rub against a stationary machinist’s flat, using
G-10.1 Place the specimen in the appropriate elec-
No. 1 to No. 000 emery or emery paper to make
trode assembly (see G-4.1.19). lower the electrodes
successive cuts. The resulting elliptical face should be
and check the spacing.
a highly polished surface inclined at 30 z lo to the axis
of the electrode. The electrodes are considered prop-
G-10.2 Lower the draft shield, close S, and adjust Ts,
erly sharpened and polished when no burrs or rough
if necessary, to obtain the required voltage across
edges are observable at 15 x magnification.
voltmeter V as established in the calibration proce-
dure.
G-8 CALIBRATION
G-10.3 Begin the test by first closing S,, S, and S,.
G-8.1 With the circuit connected as shown in Fig. 9,
Observe the indicator lamp, just after the lamp is
calibrate the test apparatus for correct voltage and
extinguished, simultaneously close S, and S,,, to
current as follows.
begin the timer and the first level of arc severity m ac-
cordance with Table 8. At the end of each minute
G-8.1.1 In making these calibrations, the operator
increase the arc severity in sequence as shown in
necessarily comes into contact with the high voltage
Table 8 until failure occurs as defined in G-2.2. At
wiringofthesecondarycircuit. It is, therefore, impera-
failure, immediately interrupt the arc current and stop
tive that the circuit be de-energized by opening S,
the interval timerbyopeningS,. Record the seconds to
before each change in connection is made.
failure.
G-8.1.2 Open Circuit Operating Voltage
G-10.4 While the test is in progress, watch the arc
Attach an electrostatic voltmeter across the secondary from a position nearly on a level with the surface of
of T,. With S, open and S,, and S, closed, initially the specimen todetcrmine ifthe arc is ‘nomtal’ [ lying
adjust the autotransformer, T, to provide an open close to the specimen with not over (l/l6 inches) 1.6
circuit operating voltage of 12 500 V. mm lift at its middle] and to observe the progression
of tracking. If the arc should ‘climb’ of flare irrcgu-
G-8.1.3 Adjustment ofSecondary Current larly, it is an indication that the circuit constants arc
incorrect.
With the correctly spaced electrodes resting on a
lava or ceramic block and with the draft shield NO’E - Craws are expelled forcibly from some insulators, thus
causing the arc to flutter, check the equipment for proper opera-
closed, close switches S,, S, and S,,. Adjust R,, to
tion in these instances by examining thr arc for quietness and
give the required current of 10 mA as indicated by maintenance of a position close to a surface such as glass 01 lava.
the milliammeter A. If the apparatus is checked for
r-f current in the secondary when the equipment is G-1 1 REPORT
first set up, the r-f thermocouple milliammctcr (SW
Note given under G-4.1.4) should also read 10 mA to G-11.1 ‘fhc report shall include the following infor-
indicate proper suppression of r-f. Open S, again and mation.
readjust T to give anopen circuit secondaryvoltage
of 12 500 9 as indicated by an electrostatic voltmeter. G-11.1.1 Type and trade name of material.
Repeat this procedure until no further adjustment is
necessary to obtain 10 mA and 12 500 V. Note the G-11.1.2 Conditions of fabrication.
reading on the voltmctcr Vat this time while the arc is
continuous at 10 mA. Maintain this voltage (typically G-l 1.1.3 Conditioning prior to test.
around 1lOto 115 V)forallsubsequentcalibrationand
testing. Next close, S,,alongwithS,,, thus placiugR1 G-11.1.4 Thickness of specimen, or if not a standard
in parallel withR,,. Adjust R2 to give au arc current o P specimen, a description of the part.
20 mA. Close S,, aud adjust b30 for a 30 mA current,
and, finally, close S,, and adlust R,,” to give a 40 tnA G-11.1.5 Electrode system used and orientation,
current. whether normal or inverted.

G.9 CONDITIONING G-11.1,6 Number of tests.

G-9.1 Condition spccinlcns prior to testing in accor-


G-1 1.1.7 Median and minimum arc resistance times.
dance with 7.2.
G-11.1.8 Special remarks, for instance buruing and
softening.
G-9.2 If the specimens have been kept at a tcmpera-
lure close to or below the dew point of the surround- G-11.1.9 Kind and amount of contamiuant, if any.

21
IS 13411: 1992
G-12 PRECISION AND BIAS severity stage generally exhibit better provision
than specimens which fail well into a given severity
G-12.1 Precision depends substantially on the com- stage.
position and thickness of the specimen, type of elec-
trodes used, and time of failure. In the latter case, G-12.2 No bias statement can be made since no
specimens which fail shortly after a change in the standard material exists for this test method.

ANNEX H
[Table 2,SINa (xii) ]
DETERMINATON OF HEAT DISTORTION TEMPERATURE
[ Adapted from IS0 75 : 1987 Method.A ]

H-O PRINCIPLE ture ranges to be used shall be covered and a correc-


tion term determined for each temperature. If the cor-
H-0.1 Determination of the temperature at which a rection term is 0.010 mm or greater, its algebraic sign
specified deflection occurs when a standard test speci- shall be noted and the term applied to each test by
men of plastics or ebonite is subjected to bending adding it algebraically to the reading of apparent
stress producing one of the nominal surface stresses deflection of the test specimen.
given in H-0.2, when the temperature is raised at a
uniform rate. H-l.2 Heating Bath
Containing a suitable liquid in which the test specimen
H-O.2 Two methods have been specified:
can be immersed to a depth of at least 50 mm. An
efficient stirrer shall be provided. The heating bath
- Method A, using a nominal surface stress of
shall be equipped with a means of control so that the
1.80 MPa; and
lrmperature can be raised at a uniform rate of 120 2 10
- Method B, using a nominal surface stress of
K/h. This heating rate shall be considered to be met if
0.45 MPa.
over every &minutes interval during the test, the tem-
perature change is 12 % 1 K.
H-l APPARATUS
The apparatus may be arranged to shut off the heat
H-l.1 Means of Application of Bending Stress automatically and sound an alarm when the specified
deflection has been reached.
The apparatus shall be constructed essentially as
shown in Fig. 15. It consists of a rigid metal frame in NOTES
which a rod can move freely vertically. The rod is I Liquid paraffin, transformer oil, glycerol and silicone oils may
provided with a weight-carrying plate and a loading be suitable liquid heat-transfer media, but other liquids ma) be
nose, The base of the frame is fitted with test specimen used. In all cases, it shall be established that the liquid chosen is
stable at the temperature used and does not aftect the material
supports; these and the vertical members of the
under test, for example, by swelling, softening or cracking. If uo
frame are made of metal having the same coefficient of suitable liquid can be found for use as a heat-transfer medium, a
linear expansion as the rod. fluidirod bed may be used as a heat-transfer medium.

2 Theresultsof the test may dcpcndon the thermal conductivity


The test spccimcn supports consists ot’ cylindrical- of the heat transfer medium.
shaped metal pieces 100 + 2 mm apart (see Fig. 15),
with their lines of contact in a horizontal plane, fitted H-l.3 Weights
to the base of the frame in such a way that the vertical
force applied to the test specimen by tbc loading nosr A set of weights shall be provided so that the test
is midway between them. The cdgcs of the supports specimen ran be loaded to the required nominal sur-
are parallel to the loading nose and at right angles to face stress, calculated according to H-4.1.
the length direction of a test specimen placed symmet- NOIT: - Ir may be necessary IO adjwt thcsc weights in 1 g
rically between them. The contact edges of the sup- increments.
ports and the loading nose are rounded tcj a radius of
3.0 ? 0.2 mm and shall be longer than the thickness 01 H-l.4 Thermometer
the test sprcimcn. Mercury-in-glass ol’ the partial immersion type, or
other suitable tenlperature-measurin instrument 01’
Unless vtrtical parts of the apparatus have the same
approprialc range and reading tn 0.S-8 C or less. Mcr-
cocfficicnt oflinearexl~aasion, the differential change
cury-in-glass thermomctres shall bc calibrated liar the
in the length of these parts introducts an error in
depth of immersion rrcluircd by H-4.2.
the reading of the apparent deflection of the test
sprcimen. A blank test shall be made 011rach appara- H-13 Deflection Measuring Instrument
tus using a test specimen made of rigid material
having a lnw coefficient of expansion. The tempera- A calibrated micrometer dial-gauge 01 other suitable

22
IS 13411: 1992

measuring instrument to measure to 0.01 mm the b is the thickness of the test specimen, in
deflection at the midpoint of the test specimen. millimetres;
NOTES h is the height of the test specimen, in
1 In certain forms of cmstructiom of the apparatus, the force F, millimetres; and
of a dial-gauge spring is dire/ted upward and therefore, de-
tracts from the downward forp applied by the mass of the
L is the measured length of span between
weighted rod, while in other forma, F, acts downward and supports, in millimetres.
augments that applied by the weighted rod. In such cases, it is
necessary to determine the ma nitude and direction ofF so as to Measure dimension5 band h to the nearest 0.1 mm and
be able 10 compensate for its f ffects accordingly (see If-4.1). dimension L to the nearest 0.5 mm.
F, varies considerably over the The effect of the mass m, of the rod that applies the
INI Ihat part of the stroke which is
testing force F shall be taken into account as contri-
to be used.
butingpart of that force. If a spring-loaded component
H-2 TEST SPECIMENS such as a dial gauge is used, the magnitude and
direction of the force F, exerted by its spring shall also
H-2.1 At least two test specilnens shall be used to test be taken into account as a positive or negative contribution
to the force F (see Notes 1 and 2 of H-1.5).
each sample. For moulding materials the test speci-
mens shall be a rectangular bar 120 + 10 mm in length, If required, the mass mw ck additional weight to be
between 3.0 and 4.2 mm in thickness (b) and between placed on the rod to produce tk required total force
9.8 and 15 mm in height (h). In case of compression F is given by the equation:
moulded test specimens, the height shall be perpen-
dicular to the direction of the moulding pressure. Fqr F = 9.91 (mW + mf) + Fs
materials in sheet form, the thickness of the test
specimen (which dimension is ordinarily the. thickness F -Fs
and hence m w = -m I
of the sheet) shall be in the range of 3 to 13 mm, 9.81
preferably between 4 and 6 mm.
where
NOTE - The test results obtained on specimens approaching
m w is the mass of the weight to be added, in kilo-
13 mm thick may be 2 10 4 K above those obtained from thin
mst specimens because of poorer heat transfer. grams;
F is the total force to be applied to the test speci-
H-2.2 The test results obtained on moulded test men, in newton;
specimen depend on the moulding conditions used in
their preparation. Moulding conditions shall be in is the mass of the rod that applies the testing
accordance with 7 (the standard for the material) or force, in kilograms;
shall be agreed upou by the interested parties.
is the force exerted by any spring-loaded com-
ponents involved, in newtons, and is a positive
H-2.3 Discrepancies in test results due tovariations in
value if the thrust of the spring is towards the
moulding conditions may be minimized by annealing
test specimen (downwards), or a negative value
the test specimens before test. Since different materi-
if the thrust of the spring is opposing the descent
als require different annealing conditions, anneal-
of the rod, or zero if no such component is
ing procedures, shall be employed only if required, by
involved.
the material standard or if agreed upon by the inter-
ested parties. The actual force applied shall be the calculated force
F 2 2.5 percent.
H-3 C~ONDITIONING
H-5 INITIAI, TEMPEKATUiW OF THI’
H-3.1 The specimens shall be preconditioned in HEATING BATH
accordance with 7.2.
H-5.1 The thermometer bulb or sensitive part of the
H-4 PHOC:EI)URE temperature-measuring instrument (H-1.4) shall be at
the same level and as close as possible to the test
H-4.1 Calculation of Force to he Applied specimen (within 10 m111)~ but not in contact with it.
The temperature of the bath shall be 20 to ?3”C at tlrc
The force F to be applied to the test specimen is start of each test, unless previous tests have ~IOWII that,
given, in newtons, by the equation: for the particular materials under test, no tsrror is
introduced by starting at other temperatures.
2 (1 Ml2
F=-
3L
whcrc H-6.1 Place a test specimen on the hupporls so that
0 is the maximum nominal surface stress in the the long axis of the specimen is pcrpcndic.ular to the
test specimen, in megapascals (that is, 1.80 supports. Apply the calculated force (H-4.1) IOgive a
when testing according to method A and 0.45 nominal surface stress of 1.80 MPa on the test speci.
when testing according to method H); 111rn. Allow the forcts to act for S nlinulrs r;scc~Note).

23
IS 13411: 1992
Then make the zero reading orsettingofthe measuring phous plastics or ebonite differ by more than 2 K, or
device and start the heating. This waiting period may those for semicrystalline materials by more than 5 K,
be omitted when testing materials that show no appre- repeat tests shall be carried out.
ciable creep during the initial 5 min.
Table 9 Standard Deflection Vs Height of
Raise the temperature of the bath at a uniform rate of Test Specimen
120 + 10 K/h. Note the temperature at which the bar
reaches the standard deflection corresponding to height ( c1a14se H-6.1 )
of the test specimen, as given in Table 9, as the Hetght of Test Spcclmn Standard Deft&ton
temperature of deflection under load at 1.80 MPa mm mm
nominal surface stress.
9.8 to 9.9 0.33
10.0 to 10.3 0.32
NOTE-The 5 minutes waiting period is provided to compensate LO.4 to 10.6 0.31
partially for the creep exhibited by some. materials at room 10.7 to 10.9 0.30
temperature when subjected to the specified nominal surface 11.0 to 11.4 0.2Y
stress. That part of the creepwhich occurs in the initial 6 minutes 11.5 IO 11.9 0.28
is usually a significant fraction of that whichoccurs in the first 30 12.0 to 12.3 0.27
minutes.
12.4 to 12.7 0.26
12.8 to 13.2 0.25
13.3 to 13.7 0.24
H-6.2 Express the temperature of deflection under
13.8 to 14.1 0.23
load of the material under test as the arithmetic mean 14.2 to 14.6 0.22
of the temperatures of deflection under load of the 14.7 10 15.0 0.21
specimens tested. If the individual results for amor-

ANNEX J
[ Table 3, Sl No. (ii) ]

DETERMINATION OF RESISTANCE TO CHEMICALS


( Adapted from IS0 175 : 1981)

J-O PRINCIPLE J-1.1.2 TestLiquids

J-0.1 Complete immersion of test specimens in a test Types of test liquids shall be decided after agreement
liquid for a specified temperature. between the interested parties.

J-O.2 Determination of their properties before and J-l.2 Test Temperatures


after immersion and, if applicable, after drying; in the
latter case, the determinations are made, if possible, J-1.2.1 Immersion Tempwttrres
one after the other on the same~spccimrns.
The preferred test temperatures arc:
J-l GENERAL REQ1JIREMENTS ANI)
a) 27 2 2*C, and
I’ROCEDIJRE
b) 70 + 2%.
J-l.1 Test Liquids
If a different temperature has to bc used in order to
J-1.1.1 Choice of Test Lipids correspond to the tempcraturc at which the plastic is
used, it shall be selected from the following prc-
If information is required about the bchaviour of a furred temperatures:
plastic in contact with a specific liquid, that liquid
shall, xs ii rule, bc used. In particular, the following lemperatures should he
uscd:O-2-27-40-55-85- lOO- 125- lSO”C,with
Industrial liquids are not gcncrally ofahsolutcly cou- a tolerance of 2 2OC on temperatures up to and iu-
stantcomposition. Whcneverpossihlc, the tcstshall be eluding 105°C and ? 3’C on tempcraturrs grcatcr
carried out in defined chemical products used on their than 10S°C and up to and including 200°C.
own as a mixture, and which are as rcprescntativc as
possible of the effect of the products under considcra- NO’W -- In the evcnf that the test is IU bc carried out at :I
tion on the plastic material conccrnrd. lemperaturc ahovc Ihc normal amhicnt conditions, it may 1%
desirable to condition another series of specimens al this ICIII-
NOTE - If making a series ot tests in a liquid of doubtful perarure for a period equal to that of the test, and IO mc:~surc
composition, it is important to rake all the samples of the liquid their prop&es after this condilioning in ordrr IO hr nhlr IO
from the same container. distinguish the elfcc& of temperature tram that ol thr liquid.

24
IS 13411: 1992

In the case of long duration tests, specimens stored in However, when several materials of the same compo-
air at 27OC may undergo a change in properties. sition are to be tested, it is permissible to put several
Preparation of an additional series of test specimens is sets of specimens into the same container.
recommended for comparison purposes.
In every case, no significant proportion of the surfaces
5-1.2.2 Measurement Temperature of the specimens shall make contact with the surface of
other specimens, with the walls of the container, or
The temperature for the determination of changes in with any weight that is used.
mass, dimensions or physical properties is 27O 5 2Oc.
If the immersion temperature is different, bring During the test, stir the liquids, for example, by rotat-
the specimen to 27OC by the procedure described ing the containers, at least once per day.
in J-1.6.3.

If the test lasts longer than seven days, replace the


J-l.3 Test Duration
liquid witbanequalamount of the original liquid every
seventh day.
The preferred test durations are:
a) 24 h for a short duration test; If the liquid is unstable (for example, sodium
b) 1 week for a standard test (particularly at hypochlorite), replace the liquid more frequently.
27OC); and
c) 16 weeks for a long duration test. If light is likely to have an influence on the action of the
test liquid, it is recommended to operate either in
If it is essential to adopt other test durations, for darkness or in defined illumination conditions.
example, if it is desired to perform tests as a function
of time or to plot the curve until equilibrium is reached, It may be necessary in certain cases (for example, if
it is recommended that the durations be chosen from there is a risk of oxidation) to specify the height of the
I he following standard scales: liquid level above the specimens.

a) 1 - 2 - 4 - 8 - 16 - 24 - 48 - 96 - 168 b, J-1.6.3 Rinsing and Wiping


b) 2-4-8-16-26-52-78weeks,and
At the end of the period of immersion, bring the
c) 1.5 - 2 - 3 - 4 - 5 years. temperature of the specimens back to ambient tem-
perature, if necessary, by transferring them quickly
J-l.4 Test Specimens
into a fresh quantity oftest liquid at room tempcraturc,
for a period of 15 to 30 minutes.
Depending upon the proposed test after exposure
(mass, dimensions, physical properties) and the nature
Remove the specimens from the test liquid and rinse
and form (sheet, film, rod, etc) of the plastic material,
tbemwitbaproductwhicb hasnoeffecton the material
the specimens will be of diverse shapes and dimen-
under test and which is chosen to suit the nature of the
sions.
test liquid.
They may bc obtained by moulding, or by machining.
Wipe the specimens dry with filter paper or a lint-free
In the latter case, cut surfaces shall be machined to a
cloth.
fine finish and shall show no trace of carboni72tion
that could be attributed to the method of preparation. NOTES

1 It requested, it may be necessary IO examine the &I liquid at


J-l.5 Conditioning
the end of the test. This examination may he a simple visual
examination or a more rigorous examirhon, incl;ding, for
Condition the specimens in accordance with 7.2. example, a tilralion.

This examination may not be practicable if the liquid has been


J- 1.6 Procedure replaced during the test.

J-1.6.1 Quanbfy ofTest Liquid 2 In the case of specimens tested in solvents such as arctone or
alcohol al ambient temperature, rinsing and wimping may not be
necessary.
The quantity of test liquid used shall be at least 8 ml
per square centimetre of the total surface area of J-l.7 Expression of Hesults
the specimen in order to avoid a concentration of
extracted product in the liquid during the course of the J-1.7.1 Numcricnl Expression
test. The test liquid shall cover the spccin~cn com-
pletely. In addition to the results of measurements bcforc and
after immersion, the results may bc cxprcsscd (cx-
J- 1.6.2 Positioning ofSpecimens cept in special casts of changes in mass) as a pcr-
centagc of the value of the property after inlnrersion
As a rule, place each of test specimens in a given (V,) with rcspcct to the value before immersion (V,),
container and completely immerse them in the ~cst that is, iis:
liquid (using a weight, if necessary).

2s
IS 13411: 1992
J-1.7.2 Graphical Expression NOTE - In certain special cases. a square spccimrn. 50 mm x
50 mm x 4 mm, may be used by agreement behven the inkrr%ted
In every case where measurements are made as a parties.

function of time, it is recommended that correspond-


ing graphs be plotted. The values obtained (includ- J-2.2.2 Slleets and Plates
ing the original value), or the differences in value,
Specimens shall be 50 f: 1 mm square and shall be
shall be plotted as the ordinates, and the durations (1)
machined from the sheet or plate submitted for test.
as the abscissae. If it is necessary to shorten the
duration scale, either a r scale or a log I scale may be
The thickness of the specimens shall be the same as
used. thaw of the sheet or plate sumbitted for test, if its
nominal thickness is less than or equal to 25 mm.
J-2 DETERMINATION OF CHANGES IN MASS
AND (OR) DIMENSIONS AND (OR)
If the nominal thickness is greater than 25 nun, and in
APPEARANCE
the absence of special provisions in the relevant
specification, reduce the thickness of the specimen to
This determinations may, if necessary, be carried out
25 mm hy machining one face only.
on the same specimens.
J-2.3 Determination of Changes in Mass
At least three specimens shall be used.
J-2.3.1 Procedtrre
J-2.1 Apparatus
J-2.3.1 .l Conditioning
J-2.1.1 Beakers
Condition the specimens and select the test conditions
Of suitable dimensions and fitted with lids (airtight, if in accordance with J-l.
necessary, and fitted with condenseIs in the case of
volatile liquids or those which give off vapoum). J-2.3.1.2 Determination of initial mass

J-2.1.2 Enclosure, thermostatically controlled at the Determine the mass m, of each specimen to the nearest
0.001 g in case of specimens of mass greater than or
test temperature.
equal to 1 g, or to the nearest 0.000 1 g in the case of
specimens of mass less than 1 g.
J-2.1.3 Thermometer, ofsuitable range and accuracy.

J-2.1.4 For Determination of Chunges in Mass Immerse the specimens in the test liquid as specified
in J-1.6.2.
J-2.1.4.1 Weighing bottle
J-2.3.1.3 Measurement immediately ufier immersion
J-2.1.4.2 Balance Place each rinsed and wiped specimen in a tared
weighing bottle, stopper it and determine the mass m,
Accurate to within 0.001 gin the case of specimens of to the nearest 0.001 g or 0.000 1 g as appropriate
mass equal to or greater than 1 g, or to within 0.000 1 (see J-2.3.1.2).
g in the case cif specimens of mass less than 1 g.
If the liquid used for the test is volatile at ambient
J-2.1.5 For Determination of Dimensionul Changes temperature, the time during which the specimen is
exposed to the air shall not exceed 30 seconds. If it is
J-2.1.5.1 Dialmicrometer, with flat anvils, accurate tv necessary to continue the test after weighing (test as a
0.01 IllIll. function of time), immediately replace the specimens
in the test liquid and put the containers back in the
J-2.1.5.2 Caliper gauge, capable of measuring to an thermostatically controlled enclosure.
accuracy of 0.1 mm.
J-2.3.1.4 Measurement after immersion and drying
J-2.1.6 Ventilated oven, if required, capable of being
controlled at the chosen drying temperature. Remove the specimens from the weighing bottles and
dry them in the oven at the specified temperalure
NOTE - In the abscncc of any spccial instructions. USC’ an wcn
(usually for 2 h at 50 + 2’C) to constant mass. Cool thr
controlled at 511 tr 2”~:.
specimens if necessary, recondition them in accor-
dance with J-2.3.1.1 and detenline the mass m, ofcal-h
J-2.2 Test Specimens (see cllso J-1.4)
specimen.
J-2.2.1 Moulding Materials

Specimens shall have a diameter of SO + 1 IIUU and a


thickness of 3 I! 0.2 mm. They shall be mouldcd to
shape under the conditions sprcified in 11~ appropri-
ate produci specification (or uudcr the cundilions
prcsrrihcd by the supplier). After rrmvval from the tesl liquid, rinse and wipe th(
IS 13411: 1992

specimens in accordance with J-1.6.3, then immedi- J-2.4 Determination of Changes in Dimensions
ately place the specimens in the oven and proceed in
accordance with J-2.3.1.4. J-2.4.1 Procedure

J-2.3.2 Calculation and Expression of Results J-2.4.1.1 Conditioning

J-2.3.2.1 Report for each specimen, the masses in Conditioning the specimens and select the test condi-
milligrams, of: tions in accordance with J-1.

a) the specimen before immersion, m,,


J-2.4.1.2 Determination of initial dimensions of test
b) the specimen immediately after Immenion
specimens
m,;
c) the specimen after immersion, drying and
reconditioning, m,. J-2.4.1.2.1 Discs

Calculate the values of: Mark and measure two mutually perpendicular
diameters to the nearest 0.1 mm by means of the
m2 - m,, caliper gauge. Record the mean I,.
and
Measure the thickness of the specimen at four refer-
mj--,, ence points to the nearest 0.01 mm by means of the
dial micrometer. Record the mean, e,.
and report these values with the applicable signs.
These points shall be situated at least 10 mm from the
J-2.3.2.2 It is permissible, subject to agreement edges of the specimen.
between the interested parties, or on request, to
express the results by the following methods. J-2.4.1.2.2 Square specimens
Mark and measure the lengths of the four sides of lbc
J-2.3.2.2.1 Method I - Change in massper unit area specimentothenearestO.lmmbymcansoftbecaliper
gauge. Record the mean, I,.
For each specimen, calculate the increase or decrease
in mass per unit area, expressed in milligrams per Measure the thickness of the specimen at four refer-
square centimetre, by means of one of the following ence points to the nearest 0.01 mm by means of the dial
formulae: micrometer. Record the mean, e,.

(m2 - m&A J-2.4.1.3 Immersion


or llullerse the specimens as indicated in J-1.6.2.
(ml - m,)lA J-2.4.1.4 Measurement immediately after immersion
where Make the same measurements on each specimen as
m,, m2, and rnJ have the same meanings as in in J-2.4.1.2. Record the mean value of I, and ez, a$
J-2.3.2.1; and appropriate.
NOTE- As a general rule, it is rccoumended non IO wait helore
A is the initial total surface area, in square commencing the dctennination of dimensions.
centimetres, of the specimen.
J-2.4.1.5 Measurement after immersion and drying
J-2.3.2.2.2 Method II - Percentage change in mass Dry the specimens in the oven at the temperature
For each specimen, calculate the pcrcentagc increase prescribed aud for the specified time (usually for 2 h
or decrease in mass by mcan~ of out of Ibc following at 502 2’C). Allow the specimens to cool, if necessary,
formulae: recouditiou them in accordance with J-2.4.1.1,
then make the same measurements on each specimen
100 (m, - m,)/m, as in J-2.4.1.2. Record the mean values 01’1, and oJ, as
appropriate.

J-2.4.1.6 Measurt~ment on1.y after immcwion l111d


100 (m, - m,)/m, drying
Immediately after immersion, remove the specimens,
where m,, m, and m, have the same meanings as
rinse and wip thwl, then place the specimrns in tbc
in J-2.3.2.1 +
OW~I and procwd as described in J-2.4.1.5.

J-2.3.2.3 111every GIST, ralculalc lbc arithmetic mean


(or means) of the results for spccimcns t;jken from the
same sample.

27
IS 13411: 1992
dimensions, express the final dimensions as percent- J-2.5.2 Expression of Results
ages ofthe initial dimensions. Calculate these percent-
Express the results using the notation scale given in
ages for each specimen, each dimension, and each
Table 10.
variation of test procedure. These percentages may be
greater than, equal to, or less than 100 percent, the
Report separately the results to specimens that have
value 100 percent signifying that the action of the
been simply immersed and wiped dry and those relat-
liquid has not changes the dimension.
ing to specimens that have also been oven-dried
and reconditioned.
J-2.4.2.2 Calculate the airthmetic mean (or means) of
the results relating to the specimens taken from the
J-3 DETERMINATION OF CHANGES IN
same sample.
PHYSICAL PROPERTIES
J-2.4.2.3 If applicable, plot graphs of the results as a
The properties investigated may be mechanical, elcc-
function of test duration.
trical, thermal or optical, etc.
J-2.5 Determination of Changes in Appearance
J-3.1 Apparatus
Examination of changes in appearance may be
conducted together with the other tests described in J-3.1.1 Apparatus specified in J-2 excluding the hal-
this standard, or may be carried out separately. In antes unless required for special cases.
every case, prepare supplementary specimens for
comparison. J-3.2 Test Specimens

J-2.5.1 Procedure J-3.2.1 Shpe nnd Dimensions


The specimens shall have the shape and dimensions
J-2.5.1.1 If the change in appearance is determined
specified in the relevant Indian Standards for the
as a complement to one of the tests specified in this
determination of the properties under consideration.
standard, use the procedure specified for that test.
If several sizes of test specimen are allowed, choose,
J-2.5.1.2 If the change in appearance is determined
in preference, the size having a thickness ncarcst to
separately, use the general procedure (see J-l) sub-
4 mm.
ject to agreement between the interesed parties.
J-3.2.2 Number
J-2.5.1.3 Examine each specimen, by means of a lens
if necessary, in comparison with an untreated Prepare the number of specimens specified in 10. In
specimen and record any change in appearance as the case of tests that alter the test specimen (in particu-
follows, using the notation scale given in Table 10 : lar, tests to destruction) prepare additional spccimcns
to serve as a control.
a) colour (including the nature of the change and
whether or not it is uniform);
J-3.3 Procedure
b) capacity; and
c) gloss or matt finish.
J-3.3.1 Conditioning
Note also, if present, the following effects:
Condition the specimens and choose the conditions 01
development of crazing and cracking; test in accordance with J-l.
development of blisters, pitting and other
similar effects; Determine the initial values of the selected physical
presence of material which can be easily properties in accordanrc with the relevant Indian
rubbed oft; Standards.
tacky appearance;
delamination, warping or other deformation; Immerse the specimens in the test liquid as indicated
and in J-1.6.2.
partial dissolution.
5-3.3.2 Measurement Immediately After Immcrsiott
Table 10 Notation Scale If the liquid used in the test is volatile at ambient
temperature, determination of the properties shall
Notation Change in Appearance conunence 2 to 3 min after removal of the spccimcus
from the liquid.
0 . . “one
NOW -As a general rule, ir is reconwended noi to wait I~ef~rc
..___ ._ ____..__._._____ ._.., <light wmmencing the determinalinn or the propcrtirs
I’

.I -3.3.3 Mellsrtwmmt AJier lmmcrsion trnd Drying


M Inodrrale
Dry the specimens in the ventilated oven, controlled at
I, . . tnrgc 11ir specified tcmpcrature, for the specified time or,
in lhr absrncr of any specification, al SO 2 2°C Ibr

28
IS 13411: 1992

2 h + 15 min. Allow the specimens to cool, if necessary V,, the values of the property for each specimen
and recondition them in accordance with J-3.3.1. immediately after immersion; and
NOTE - In certain cases, the interested parties may agree that
the plastics under test require no conditioning. V , the values of the property for each specimen
a r ter immersion, drying and reconditioning.
Redetermine the values of the selected physical
properties in accordance with the relevant Indian J-3.4.2 For measurable properties (that is, those for
Standards. which the measurement scale is proportional), calcu-
late the final percentage value of this property with
-J-3,3.4 Measurement Only A&r Immersion and Drying respect to the initial value by the respective formulae:

Immediately after immersion, remove the specimen, (VjV,) x la,


rinse and wipe them, then place the specimens in the
drying oven and proceed in accordance with J-3.3.3. or
<V,lV,> x loo
J-3.4 Calculation and Expression of Results
These percentages may be greater than, equal to, or
J-3.4.1 Calculate the values of the physical properties less than 100 percent, the value 100 percent signifying
as specified in the relevant Indian Standards. that the section of the liquid has not affected the
Calculate the average values of: property concerned.

V,, the values of the property for each specimen J-3.4.3 If applicable, plot graphs of the results as a
before immersion (or of the control specimen); function of test duration.

ANNEX K
[Table 3, Sl No. (iv) ]
DETERMINATION OF COEFFICIENT OF LINEAR THERMAL EXI’ANSlON
( Adapted from ASTM D 696-79 )

K-O SUMMARY K-l.2 The nature ofmost plasticsand thcconslruction


of the common type of dilatometer make -30 IO t
This test method is intended to provide a mran.. ot 30°C (-86OF to t X6OF) a convcnicnt tcmpcraturc
determining the coefficient of linear thermal cxpan- range for linear thermal expansion measurcmcnts
sion of plastics which are not distorted or indcntcd by of plastics. This range covers the temperatures in
the thrust of the dialtometer on the specimen. The which plastics are very commonly used. When
specimen is placed on the bottom of the outer dial- cxtcnding lbc range or when the n~easurellleilt of a
tometer tube with the inner or resting on it. The plastic whose characteristics are not known through
measuring device which is firmly attached to the outer the standard range is being made, particular
tube is in contact with the top of the inner tube and attention shall be paid to the factors like changes in
indicates variations in the length of the specimen with moisture rontcnt, curing, loss of plasticizers, or
changes in temperature. TemperdluK’ changes an: brough! solvents, release of stresses, phase rhangrs, elc, and
about by immersing the outer tube in a liquid bath at special preliminary investigations by thermo-
the desired temperature. mechanical analysis forthc location ofphasr changes,
may be required to avoid excessive error. Other ways
K-l SIGNIFICANCE AND 1TSE of locating phase cbangcs or transition temperature
K-l.1 The coefficient oflinear thermal cxpan~ion, cl, using the dilatomclcr itself may be employed to
between temperature T, and T2 for a specimen wbos~ cover the range of temperature in question by using
length is co at the reference temperature, is given by smaller steps than 30°C (86°F) or by observing the
the followmg equations: rate of expansion during a steady rise in tcnlperaturc
of the specimen. Once such a transition point 11;)s
a = (L2 - L,) /IL, (T, - T,) ] = AL/L, AT been located, a separate cocfficicnt of cxpanGon for
where a tcmpcraturc mllge below alId above the tralisilion
poini shall be determined. For specification and
,!,, and L, are the specimrn lr~lg:lh\ 81 comparison )utp”Srs, thr range rroni -30°C to
temperatures T1 and T,, rcsprctivcly, (1 is, +3O”C (-86 d F to +86”F) (provided it is known IlliiI
thercforc, obtamcd by dividing the linear no transition point exists in this range) shall IK
rxpansian per unit length by the change in used.
temperature.

20
IS 13411: 1992
K-2 APPARATUS and the more sensitive the measuring device, the more accurate
will be the determination if Ihe temperature is well conlrolled.

K-2.1 Fused-Quartz-Tube Dilatometer


K-4.3 The cross section of the test specimen may be
A clearance of approximately 1 mm is allowed between round, square, or rectangular and should fit easily
the inner and outer tubes. into the outer tube of the dilatometer without exces-
sive play on the one hand or friction on the other.
K-2.2 Device - for measuring the changes in length The cross section of the spccimcn shall be large
(dial gauge, LVDT, or the equivalent) shall be fixed on enough so that no bending or twisting of the specimen
the mounting fixture so that its position may be occurs. Convenient specimen cross sections are 12.5
adjusted to accommodate specimens ofvarying length by 6.3 mm (l/2 inches by 1/4 inches), 12.5 by 3 mm
(see K-4.2). The accuracy shall be such that the error (l/2 by l/8 inches), 12.5 mm (l/2 inches) in diamrter
of indication will not exceed f 1.0 pm (4 x 10’ inches) or 6.3 mm (l/4 inches) in diameter. If excessive play
for any length change.‘The weight of the inner silica is found with some of the thinner specimen, guide
tube plus the measuring device reaction shall not sections may be cemented or otherwise attached IO
exert a stress of more than 70 kPa (10 psi) on the the sides of the specimen to fill out the space.
specimen so that the specimen is not distorted or
appreciably indented. K-4.4 The ends of the specimens shall be reasonably
flat and perpendicular to the length axis of the
K-2.3 Scale or Caliper specimen. The ends shall be protected against, indcn-
tation by means of flat, thin steel plates cemented or
Capable of measuring the initial length of the speci- otherwise firmly attached to them before the spcci-
men with an accuracy of + 0.5 percent. men is placed in the dilatometer. These plates shall bc
0.3 to 0.5 mm (0.012 to 0.020 inches) in thickness.
K-2.4 Liquid Bath - to control the temperature of
the specimen. The bath shall be so arranged that K-5 CONDITIONING
uniform temperature over the length of the specimen
is assured. Means shall be provided for stirring the K-5.1 Conditioning
bath and forcontrollingits temperature within + 0.2’C
(2 0.4OF) at the time of the temperature and measuring Condition the test specimen at 27 + 2OC and 65 + 5
device readings. percent relative humidity for not less than 40 h prior
to test. In cases of disagreement, the tolerances shall
NOTE - II is preferable and not difficult 10 avoid contact br + l°C and 2 2 percent relative humidity.
between the balh liquid and the tesl specimen. If such contact is
unavoidable, care must be taken to select a liquid Lhat will nol
affect the physical properties of the material under fest. K-5.2 Test Conditions

K-2.5 Thermometer or Thermocouple - The bath Conduct tests in the Standard Laboratory Atmos-
temperature shall be measured by a thermometer phcrc of 27 + 2OC (73.4 2 3.6”F) and 65 + 5 percent
or thermocouple capable of an accuracy of 2 O.l’C relative humidity, unless otherwise spccificd in the
(” 0.2OF). trst methods or in this specification. In cases of dis-
agreement, the tolerances shall bc + 1°C and + 2
K-3 SAMPIJNG percent rclativc humidity.

Unless otherwise agreed upon between intcrestcd K-6 I’HOCEDIJIW


parties, the material shall be sampled according to 10.
K-6.1 Measure the length of the conditioned spcci-
K-4 TES1’ SPECIMENS men at room tcmpcraturc to the nearest 25 elm (0.001
inches) with the scale or caliper (sL’~ K-2.3).
K-4.1 The test specimens may be prepared by
machining, moulding, or casting operations under K-6.2 Ccmcnt or otherwise attach ‘the steel plates
conditions which have a minimum of strain or to the ends of the specimen to prevent indentation
anisotropy. If specimens are cut from samples that are (see K-4.4).
suspected of anisotropy, the specimens shall be cut K-6.3 Mount the specimen in the dilatometcr.
along the principal axes of anisotropy and the Carefully install the dilatometrr in the -30°C (-22°F)
coefficient of linear expansion shall be measured on bath so that the top of the spccimcn is at least SO II~IH
each set of specimens. (2 inches) below the liquid Icvcl of the bath. Maintain
the temperature of the bath in the range I’rom -32°C
K-4.2 The specimen length shall bt between 50 mm to 2H”C (-25 to -18°F) t 0.3”C (O.J”F) until thr
(2 inches) and 125 mm (5 inches). tcmpcraturr of the spccinicn reaches the tcmpcra-
turn of the bath as dcnotcd by 110 further movrm~n~
NOTE - If specimens shorter lhan 50 mm (2 inches) arc used. a indicated by the mcasuringdrvicc over ;I period 01’5 to
lozs in sensirivily results. It spcrimcns grcally longer lhan 125
10 minutes. Record the actual temperature and the
mm (5 inches) are used. rhe temperalure pradienr along the
specimen becomes difficult IO confrol within the prescribed
measuring device reading.
Irmits. The length used will be govcrncd by the scnsilivity and
rangeof the measuring device, the exlension expected and lhc
K-6.4 Without disturbing or jarring the clilalonlcl~r,
accuracy d&red. Gcncrally speaking. Ihe longer the spccimcn rhauge to the +3O”C (+86”F) bath. so &II the ION,01’

30
IS 13411 : 1992
the specimen is at least 50 mm (2 inches) below the ancy shall be investigated and, if possible, eliminated.
liquid level of the bath. Maintain the temperature of The test shall then be repeated until agreement is
the bath in the range from +32 to +28OC (+82 to 90°F) reached.
+ 0.2OC (2 0.4OF) until the temperature of the speci-
men reaches that of the bath as denoted by no further K-7 CALCULATION
changes in the measuring device reading over a
period of 5 to 10 minutes. Record the actual tcmpera- Calculate the coefficient of linear thermal expansion
ture and the measuring device reading. over the temperature range used as follows:
a =ALfLo AT
K-6.5 Without disturbing or jarring the dilatometer,
change to the -3OOC (-22OF) bath and repeat the where
procedure in K-6.3. .
a coefficient of linear expansion per degree Ccl-
NOTE - It is convenient IO use alternately IWO baths at the sius;
proper temperatures. Great care should be taken not to disturb
the apparalus during the transfer of baths. Tall Thermos bottles
AL change in length of test specimen due to heating
have been successfully used. The use of IWO baths is preferred or to cooling;
because this will reduce the lime required to bring the specimen
L” length of test specimen at room temperature
to the desired lemperature. The test should be conducted in as ( AL and L, being measured in the same units);
short a lime as possible to avoid changes in physical properties
during long exposures IO high and low temperatures that might
and
possibly take place. AT temperature differences, OC, over which the
change in the length of the specimrn is meas-
K-6.6 If the change in length per degree of tempera- urcd.
ture difference due to heating does not agree with
the change in length per degree due to cooling within The values of for heating and for cooliug shall bc
10 percent of their average, the cause of the discrep- averaged to give the value to be reported.

31
1s 13411:1992

r~ TfUKit4G U)GE

—.—
.
om8io.2
1

“’”0”’-7----%
\
E 7 (-4
o’

COMTACT WITjI THE


SpU21htEN ANI) PARAILCL
ICI WITHIN 0.025 mm

~o 2 VICE $LTFWT AND ‘iksT%’ECME!!( ~0’CCHAM! STmK1.No


moE
SHOW W ~OitMAL %SI’RON )

\ RA~iuS OF NOTCH ‘tlASL


y~ =o.8y o.2sk cl{05mfn

F[ci. 3 TYPEA NOTCH

33
IS13411:1992

RADIUS OF NOTCH BASE


1.of 0.05

FIG.
4 TYPE B NOTCH

+s
\ DIRECTION OIRECTION
OF BLOW OF BLOW

\+
2,
FIG. 5 NOTCHEDTESTSPECIMENPY)RLAMINATED
Smx T%STEDM THE FLATWISED~RIXXON

34
‘Y 6

-c

——. ._
Q

Op

WIDTH OIRECTION
c lHE PRODUCT

FIG. 7 POSITION
OF T%T PIECEIN RELATION
TO
LENGTHANDWIDTHOF SHEET

I 1

b
L

—,.
l+
APPLIID LOAD

——
“--l

II

FM. 8 POS1”IION OF ~N PIECE D[rRIN(; ~kS’r

35
IS 13411: 1992

2-l
SPEC’MEN
d\
X
R, 15ooon
A

LJ
1.2 TO 1.5 HENRIES
(SEE TEXT)

I I
_! I
I7 4
115 v
T” l c 1

NOTE -Switches Sm to S,, are aligned in the sequence of their closing. from brrom to top, during a test.

FIG. 9 ARC-kWTAtWE TEST CIRCUfT

36
IS 13411: 1992

i. 10 GRLWIIING
AND POLISHINGBLOCKWI’IHTUNWIXN Ron E~.ECTRODES
INPLACI:

FIG 11 Tw ANI) Sm VIEWS OF T~JNGSRNRoe EI_ECIROL)I:

37
IS 13411: 1992

:I
- 16.5 __c
L’2.7--.
-II- 0.254+0.025

,- COUNTERSUNK
I-
n
4
CLEARANCE FOR
4-40
MACHINE
FLAT HEAD
SCREW I
TAPPED FOR
4-40 SCREW

SET SCREW

NOTE - The 0.025 mm, SIOIand the corresponding angled comer mast be made IO provide a left and right holder.

All dimensions in millimetres.

FIG. 12 HOLDER DETAIL

-----__
@
,c, I_-
--Iq t j /
@ I
I8

FIG 13 STRIP EJ.KTR~DI: HOLDER ASSPMULY

38
Standard Mark

The use of the Standard Mark is governed by the provisions of the Bureau of Indian
Stand(rrds Act. 1986 and the Rules and Regulations made thereunder. The Standard Mark on
products covered by an lndian Standard conveys the assurance that they have been produced
to comply with the requirements of that standard under a well defined system of inspection,
testing and quality control which is devised and supervised by BIS and operated by the
producer. Standard marked products are also continunusly checked by RI’S f(w conformity
to that standard as a further safeguard. Details of condtrinns under which a licence for the
use of the St:lndard Mark m:\y be granted to manufacturers or producers may be obtained
from the Bureau of Indian Standards.
Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote
harmonious development of the activities of standardization. marking and quality certification of goods
and attending to connected matters in the country.

Copyright

BIS has the copyright of all its publications. No part of these publications may be reproduced In
any form without the prior permission in writing of BIS. This does not preclude the free use, in the
course of implementing the standard, of necessary details. such as symbols and sizes, type or grade
designations. Enquiries relating to copyright be addressed to the Director ( Publications ). BIS.

Revision of Indian Standards

Indian Standards are reviewed periodically and revised, when necessary and amendments, if any, are
issued from time to time. Users of Indian Standards should ascertain that they are in possession of
the latest amendments or edition. Comments on this Indian Standard may be sent to BIS giving the
following reference :

Dot : No. PCD 12 ( 751 )

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

BUREAU OF INDIAN STANDARDS

Headquarters:

Manak Bhavan, 9 Bahadur Shah Zafar Marg, New Delhi 110002


Telephones : 331 01 31. 331 13 75 Telegrams : Manaksanstha
( Common to all Offices 1

Regional Offices: Telephone

Central : Manak Bhavan, 9 Bahadur Shah Zafar Marg 331 01 31


NEW DELHI 110002 331 13 75

Eastern : l/l4 C. I. T. Scheme VII M. V. 1. P. Road. Maniktola 37 84 99, 37 85 61,


CALCUTTA 700054 37 86 26, 37 86 62

Northern : SC0 445-446. Sector 35-C. CHANDIGARH 160036 53 38 43, 53 16 40,


{ 53 23 84
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Branches : AHMADABAD, BANGALORE, BHOPAL, IIHUBANESHWAR, COIMBATORE.


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hinted at Pr-intrade, New Delhi, India

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