Methods For Testing Tar and Bituminous Materials - Determination of
Methods For Testing Tar and Bituminous Materials - Determination of
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ICS 75.140
© BIS 2021
FOREWORD
This Indian Standard (Second Revision) was adopted by the Bureau of Indian Standards after the draft finalized by
the Bitumen, Tar and Related Products Sectional Committee, PCD 06 had been approved by the Petroleum, Coal
and Related Product Division Council.
This standard was originally published in 1958 as ‘Methods for testing tar and bituminous materials —
Determination of flash point and fire point’ and first revised in 1978. ‘Methods for testing tar and bituminous
materials’ was originally published as series of 22 standards in the form of a booklet, as listed below:
Sl No. IS Designation Title
1. IS 1201 : 2004 Sampling
2. IS 1202 : 1978 Determination of specific gravity
3. IS 1203 : 1978 Determination of penetration
4. IS 1204 : 1978 Determination of residue of specified penetration
5. IS 1205 : 1978 Determination of softening point
6. IS 1206 (Part 1) : 1978 Determination of viscosity: Part 1 Industrial viscosity
7. IS 1206 (Part 2) : 1978 Determination of viscosity: Part 2 Absolute viscosity
8. IS 1206 (Part 3) : 1978 Determination of viscosity: Part 3 Kinematic viscosity
9. IS 1207 : 1978 Determination of equiviscous temperature (EVT)
10. IS 1208 : 1978 Determination of ductility
11. IS 1209 : 1978 Determination of flash point and fire point
12. IS 1210 : 1978 Float test
13. IS 1211 : 1978 Determination of water content dean and stark method
14. IS 1212 : 1978 Determination of loss on heating
15. IS 1213 : 1978 Distillation test
16. IS 1214 : 1978 Determination of matter insoluble in benzene (withdrawn due to
toxic nature of benzene)
17. IS 1215 : 1978 Determination of matter insoluble in toluene
18. IS 1216 : 1978 Determination of solubility in carbon disulphide trichloroethylene
19. IS 1217 : 1978 Determination of mineral matter ash
20. IS 1218 : 1978 Determination of phenols
21. IS 1219 : 1978 Determination of naphthalene
22. IS 1220 : 1978 Determination of volatile matter content
However, the Committee responsible for the formulation of standards in the field of bitumen, tar and related products
decided to publish these Indian standards separately for each test so as to make it user friendly. Accordingly,
second revision of the standard, IS 1209 Methods for testing tar and bituminous materials — Determination of
flash point and fire point ‘was taken up to formulate individual standard.
In this revision all the amendments issued earlier have been incorporated and technical modifications are not
introduced.
The Composition of the Committee responsible for formulation of this standard is given at Annex A.
In reporting the results of a test or analysis made in accordance with this standard, if the final value, observed or
calculated, is to be rounded off, it shall be done in accordance with IS 2: 1960 ‘Rules for rounding off numerical
values ( revised )’.
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IS 1209 : 2021
Indian Standard
METHODS FOR TESTING TAR AND BITUMINOUS
MATERIALS — DETERMINATION OF
FLASH POINT AND FIRE POINT
( Second Revision )
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rim, shall be not less than 0.8 mm and not more 3) Shutter — The lid shall be equipped with
than 2 mm. There shall be a proper locating a brass shutter, approximately 2.5 mm in
device, engaging with a corresponding locating thickness, operating on the plane of the upper
device on the flange of the cup. There shall be surface of the lid. The shutter shall be so
four openings in the cover (see Fig. 2) with the shaped and mounted that it rotates on the axis
following dimensions: of the horizontal centre of the lid between the
i) Opening A is an area defined by arcs of two stops, so placed that when in one extreme
two concentric circles and the intersected position, the openings A, B and C of the lid
lengths of two radii. The radius of the are completely closed and when in the other
outer circle shall be not less than 22.4 mm extreme position, these orifices are completely
and not more than 24.6 mm. The radius opened.
of the inner circle shall be not less than 4) Flame-exposure device — The flame-exposure
13.5 mm and not more than 14.2 mm. The device shall have a tip with an opening
chord of the arc of the outer circle shall be 0.7 to 0.8 mm in diameter. The flame exposure
not less than 12.7 mm and not more than device shall be equipped with an operating
13.7 mm. mechanism which, when the shutter is in the
ii) Openings B and C are of equal areas, each open position, depresses the tip so that the
of the same general form as opening A, but centre of the orifice is between the planes of
of approximately half the (angular) width. the under and upper surfaces of the lid proper,
The radii of the defining inner and outer at a point on a radius passing through the centre
circles shall be within the limits specified of the larger opening A and approximately
for the radii of the two circles, arcs of 2.5 mm from the outer edge of the opening.
which partly define opening A. The chord A pilot flame for automatic relighting of the
of the outer arc for opening B or opening exposure flame should be provided. A bead,
C shall be not less than 4.8 mm and not 4 mm in diameter of suitable material, may
more than 5.6 mm. The sum of the areas of be mounted on the lid so that size of the
openings B and C shall be neither less than test-flame can be regulated by comparison.
75 percent, nor more than 100 percent of The mechanism operating the shutter should
the area of opening A. Openings B and be of the spring type and constructed so that
C shall be equally distant from opening when at rest the shutter shall exactly close the
A and radii drawn through each of their three openings A, B and C. When operated to
centres shall be at an angle of not less than the other extreme, the three openings in the lid
135° and not more than 140°. shall be exactly open and the tip of the exposure
tube shall be fully depressed. If the air bath is
iii) Openings A, B and C need not conform
electrically heated and gas is not available,
exactly to the shape of geometrical figures
an oil burner shall be used to provide the
bounded by arcs of two concentric circles
test-flame, the position of which shall
and intersected lengths of radii. Their
correspond with that of the gas flame
boundaries should, however, fall on or
previously specified.
between the lines indicated by the limiting
values of the dimensional specification of c) Stove — Heat shall be supplied to the cup by means
the preceding text and of Fig . 2. of a properly aligned stove which is equivalent to
an air bath. This stove shall consist of (1) an air
iv) Opening D is a split tube to grip
bath, and (2) a top plate on which the flange of the
the thermometer collar. Its centre is
cup rests.
approximately 20 mm from the centre
of the lid and on a radius at an angle of 1) Air bath — The air bath shall have a cylindrical
not less than 50° and not more than 60° interior, 41.3 to 42.2 mm in depth and a
to a radius passing through the centre of diameter not less than 3 mm and not more than
opening C. It shall be set at an angle of 4 mm greater than the outside diameter of the
not less than 10°, and not more than 15° cup . The air bath may be either a flame-heated
to the perpendicular. Its height shall be metal casting or an electric-resistance element.
such that when a standard thermometer is If the heating element is a flame-heated metal
in position, the bottom of the bulb shall be casting, it shall be so designed and used that
35.6 to 40.6 mm below the level of the rim the temperature of the bottom and walls is
of the cup (which corresponds to the lower approximately the same. On this account it
surface of the portion of the lid inside should be not less than 6 mm in thickness. The
the rim). casting shall be designed so that products of
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IS 1209 : 2021
combustion of the flame cannot pass up and Either of the thermometers may be employed if
come in contact with the cup. If the air bath the indicated reading falls within 93 to 110 °C.
is of the electric-resistance type, it shall be The thermometers shall be mounted securely in a
constructed so that all parts of the interior thermometer collar so that the distance from the
surface are heated equally. This necessitates underside of the rim of the collar to the bottom of the
an even distribution of resistance wire to bulb is 52 to 55 mm. The thermometer collar shall have
cover the bottom and walls, and a method of an outside diameter of 12.70 ± 0.05 mm and a flange
construction such that heat is given out from of 2.3 to. 2.8 mm in thickness. The cement used to
the whole core of the resistance element rather fasten the thermometer into the collar shall be of such
than directly from the wire. a nature that it will withstand the action of oil up to the
The result obtained with the electrically heated highest temperature at which the thermometer is used.
instrument shall agree with that obtained with A swelling shall be provided to ensure the location of
gas-heated apparatus within 1 °C and 3 °C the thermometer collar at the correct point.
respectively, according to whether the low or 4.2 Procedure
high range thermometer is used.
2) Top plate — The top plate shall be of metal. 4.2.1 Clean and dry all parts of the cup and its
The total distance from the upper surface of the accessories thoroughly before the test is started. Take
plate to the bottom of the air bath shall exceed particular care to avoid the presence of any solvent
the distance from the under surface of the used to clean the apparatus after a previous test. Fill
flange to the bottom of the cup by not less than the cup with the material to be tested up to the level
1.6 mm and not more than 3 mm. The top plate indicated by the filling mark. Place the lid on the cup
shall be mounted with an air-gap between it and set the latter in the stove. Take care that the locating
and the air bath. The top plate may be attached devices are properly engaged. Insert the thermometer,
to the air bath by means of three screws and high or low range, as required.
spacing-bushings. The spacing-bushings
4.2.2 Light and adjust the test-flame so that it is of the
should be of proper thickness to define the
size of a bead of 4 mm in diameter. Apply heat at such
air-gap which shall be not less than 3 mm nor
a rate that the temperature recorded by the thermometer
more than 4.8 mm. The spacing-bushings shall
increases between 5 to 6 °C per minute.
be not more than 9.5 mm in diameter.
d) The thermometers conforming to the following Turn the stirrer at a rate of approximately 60 revolutions
requirements shall be used: per minute. Apply the test-flame at each temperature
reading which is a multiple of 1 °C up to 104 °C.
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For the temperature range above 104 °C, apply the 5.2 Procedure
test-flame at each temperature reading which is a Bring the material to be tested and the tester to a
multiple of 2 °C, the first application of the test-flame temperature of 17 °C lower than the expected flash
being made at a temperature at least 17 °C below the point. Completely fill the air space between the cup and
actual flash point. Apply the test-flame by operating the interior of the air bath with water at the temperature
the device controlling the shutter and test-flame burner of the tester and material. Raise the temperature
so that the flame is lowered in 0.5 seconds, left in its throughout the duration of the test at a rate of not less
lowered position for one second, and quickly raised to than 1°C and not more than 1.5 °C per minute. Proceed
its high position. Discontinue the stir ring during the as described in 4.2.2 except that :
application of the test-flame.
a) Rate of heating to be not less than 1 °C and not
4.3 Calculation more than 1.5 °C per minute,
b) The rate of stirring to be 70-80 rev/min, and
4.3.1 Observe and record the barometric pressure.
c) The test-flame to be applied at each 0.5 °C rise in
4.3.2 No corrections shall be made except in case of temperature.
dispute, when the flash point figure shall be corrected
according to the following rules: 5.3 Calculation and Report
a) For each 25 mm below 760 mm barometric Calculate and report the flash point as described under
reading, add 1 °C to the flash point; and 4.3 and 4.4.
b) For each 25 mm above 760 mm barometric 5.4 Precision
reading, subtract 1 °C from the flash point.
Duplicate tests shall not differ by the limits specified
4.4 Report in 4.5.
Unless otherwise specified, normally the flash 6 METHOD C (PENSKY-MARTENS -OPEN),
point shall be taken as the temperature read on the FOR DETERMINATION OF OPEN FLASH
thermometer the time of the flame application that POINT AND FIRE POINT
causes a distinct flash in the interior or of the cup.
4.5 Precision 6.1 Apparatus
The duplicate test results should not differ by more than The standard Pensky-Martens Tester and thermometers
the following: as prescribed in Method A (see 4.1.1) shall be used
with the following modifications:
Flash Point Repeatability Reproducibility The cover of the cup shall be replaced by a clip
104 °C and below 2 °C 3.5 °C which encircles the upper rim of the cup and carries
Above 104 °C 5.5 °C 8.5 °C the thermometer and test-flame. The tube carrying
the thermometer shall have its centre on a radius at
4.6 Precautions approximately 90o to the radius passing through the
point of attachment of the test-flame, and shall be of
4.6.1 The test-flame will neither be larger than stipulated such a height that when the thermometer is in position,
nor will it be applied more frequently than specified as its bulb shall be in the vertical axis of the cup and
the surface layer is liable to be superheated. 12 mm below the filling line. The test-flame shall be
fixed at the vertical axis of the cup and in level with the
4.6.2 The bluish halo that sometimes surrounds the
upper edge of the cup.
test-flame shall not be confused with the true flash.
6.2 Procedure
5 METHOD B (PENSKY-MARTENS - CLOSED),
FOR DETERMINATION OF FLASH POINT 6.2.1 All parts of the cup and its accessories shall be
FOR CUTBACK BITUMEN thoroughly cleaned and dried before the test is started.
Particular care shall be taken to remove all traces of
5.1 Apparatus solvent used to clean the apparatus.
5.1.1 Flash Point Tester — Pensky-Martens Closed 6.2.2 The cup shall be filled with the material to be
Tester as described under 4.1.1 except that the stirrer tested up to the level indicated by the filling mark.
shall be mechanically operated to stir in a downward
direction at a speed of 70 to 80 rev/min. 6.2.3 The clip carrying the thermometer and test-flame
shall be placed on the cup and the latter set in the
5.1.2 Thermometer — Low range thermometer as stove. Care shall be taken to have the locating devices
specified in 4.1.1(d). properly engaged. The thermometer shall be inserted.
If it is known that the material will flash above 104 °C,
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higher range thermometer shall be used. Otherwise, it 6.3.2 Fire Point — The heating shall be continued until
is preferable to start with the lower range thermometer the oil ignites and continues to burn for 5 seconds. The
and change if a temperature of 104 to 110°C is reached. temperature of the material, when this occurs shall be
recorded as the fire point.
6.2.4 The test-flame shall be lighted and adjusted so
that it is of the size of a bead 4 mm in diameter. 6.4 Precision
6.2.5 Heat shall be applied at such a rate that the The following criteria should be followed for the
temperature recorded by the thermometer increases acceptability of test results:
neither less than 5°C nor more than 6 oC per minute. Repeatability Reproducibility
The surface of the material shall be carefully observed
during heating. Flash point 8 °C 11 °C
Fire point 8 °C 14 °C
6.3 Report
6.5 Precaution
6.3.1 Open Flash Point — The open flash point shall
be taken as the temperature when a flash first appears at Care shall be taken to shield the apparatus from
any point on the surface of the material. draughts.
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ANNEX A
( Foreword )
COMMITTEE COMPOSITION
Bitumen,Tar and Related Products Sectional Committee, PCD 06
Organization Representative(s)
CSIR-Central Road Research Institute, New Delhi Prof Satish Chandra (Chairman)
Airports Authority of India, New Delhi Shri Suprio Gosh
Shri Vinod Kumar Sharma (Alternate)
Bharat Petroleum Corporation Limited, R & D Ms Sonal Maheshwari
Centre,Noida
Bharat Petroleum Corporation Limited, Mumbai Shri C. Shanmuganathan
Bharat Petroleum Corporation Limited, Kochi Shri Adalazhagan K.
Refinery
Birla Institute of Technology and Science, Pilani Shri Sridhar Raju
CSIR-Central Building Research Institute, Roorkee Ms Rajani Lakhani
CSIR-Central Road Research Institute, New Delhi Dr Ambica Behl
CSIR-North East Institute of Science and Technology, Dr Shashi D. Baruah
Jorhat Dr B. P. Baruah (Alternate)
Central Public Works Department, New Delhi Shri Divakar Agrawal
Chennai Petroleum Corporation Limited, Chennai Shri H. Ramakrishnan
Dr V. Selvavathi (Alternate)
Dilip Buildcon Limited, Bhopal Shri B. B. Kameswara Rao
Shri Anush K. C. (Alternate)
Directorate General Border Roads, New Delhi Shri Umakant Kumar
Shri Ashok Kumar (Alternate)
Directorate General of Quality Assurance, Ministry of Shri Vivekanand
Defence, New Delhi Shri Anil Kumbhare (Alternate I)
Shri Sachin Vinayak Zope (Alternate II)
Engineer in Chief Branch, New Delhi Shri O. P. Srivatava
Shri R. Jayaprasad (Alternate)
G R Infra-Projects Limited, Gurugram Shri U. C. Gupta
GP Global Asphalt Private Limited, New Delhi Shri Rajesh Kumar Jain
Highways Research Station, Chennai Shri T. S. Sundar
Shri R. Geetha (Alternate)
Hindalco Industries Limited, Mumbai Shri Harshad Kumar Pandit
Hindustan Colas Private Limited, Mumbai Shri K. G. Ranganatha
Shri T. K. Subhaash (Alternate)
Hindustan Petroleum Corporation Limited Shri B. Ravi
(HP Green R & D Center), Bengaluru Shri K. R. Krishna (Alternate )
Hindustan Petroleum Corporation Limited, Mumbai Shri Santosh Dhaku Bhogale
Indian Institute of Petroleum, Dehradun Shri Manoj Srivastava
Dr Kamal Kumar (Alternate)
Indian Institute of Technology Bombay, Mumbai Dr Dharamveer Singh
Indian Institute of Technology Delhi, New Delhi Dr Aravind Swamy
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Organization Representative(s)
Member Secretary
Shrimati D. Uma
Scientist ‘D’ (PCD), BIS
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should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of
‘BIS Catalogue’ and ‘Standards: Monthly Additions’.
This Indian Standard has been developed from Doc No.: PCD 06 (16871).