Loss On Heating of Oil and Asphaltic Compounds: Standard Test Method For

Designation: D 6 – 95 American Association State
Highway and Transportation Officials Standard

AMERICAN SOCIETY FOR TESTING AND MATERIALS AASHTO No.: T47
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for

Loss on Heating of Oil and Asphaltic Compounds1
This standard is issued under the fixed designation D 6; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript
epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope (180°C). During the tests for compliance to Specification

1.1 This test method covers the determination of the loss in E 145 requirements, the oven shelf, properly placed shall be in
mass (exclusive of water) of oil and asphaltic compounds when place and rotating. In addition, it shall also comply with the
heated as hereinafter prescribed. following requirements:
1.2 The values in inch-pound units are to be regarded as 5.1.1 Construction (Note 1)—The oven shall be rectangular
standard. The values in parentheses are for information only. with minimum interior dimensions of 13 in. (330 mm) in each
1.3 This standard does not purport to address all of the direction. The oven shall have in front a tightly fitting hinged
safety concerns, if any, associated with its use. It is the door, which shall provide a clear opening substantially the
responsibility of the user of this standard to establish appro- same as the interior height and width of the oven. The door
priate safety and health practices and determine the applica- may contain a window with dimensions of at least 4 by 4 in.
bility and regulatory limitations prior to use. (100 by 100 mm), and with two sheets of glass separated by an
air space, through which a vertical thermometer located as
2. Referenced Documents specified in Section 8, may be read without opening the door;
2.1 ASTM Standards: or the oven may be provided with an inner glass door, through
D 5 Test Method for Penetration of Bituminous Materials2 which the thermometer may be observed on opening the outer
E 1 Specification for ASTM Thermometers3 door momentarily. The oven shall be adequately ventilated by
E 145 Specification for Gravity-Convection and Forced- convection currents of air and for this purpose shall be
Ventilation Ovens4 provided with openings for the entrance of air and for the exit
of heated air and vapors. Openings may be of any size and
3. Summary of Test Method arrangement provided the requirements of Specification E 145,
3.1 Fifty grams of material, spread out in a dish 55 mm in Type I, Grade B, are met.
diameter, is heated in moving air for 5 h at 325°F (163°C) and 5.1.2 Rotating Shelf—The oven shall be provided with a
the percent loss of mass determined along with a comparison, circular metal shelf having a minimum diameter of 9.8 in. (250
before and after, of any other desired characteristics. This test mm). (A recommended form of aluminum shelf is shown in
method provides only a relative measurement of the volatility Fig. 1.) The shelf shall be suspended by a vertical shaft and
of a material under test conditions. centered with respect to the horizontal interior dimensions. The
shelf shall be provided with a mechanical means of rotating it
4. Significance and Use at the rate of 5 to 6 rpm. The shelf shall be vertically located
4.1 This test method is useful in characterizing certain as close to the center of the oven as permitted by compliance
petroleum products by the determination of their loss of mass with the requirements of 7.2 regarding thermometer placement.
upon heating under standardized conditions. NOTE 1—Continued use of existing smaller ovens complying with the
requirements of this test shall be permitted for an indefinite period to
5. Apparatus provide for normal amortization of present equipment. However, all new
5.1 Oven—The oven shall be electrically heated and shall ovens purchased should comply with the minimum dimensions and
conform to the performance requirements of Specification requirements of this test method.
E 145 Type I, Grade B, for operating temperatures up to 365°F 5.2 Thermometer—An ASTM Loss on Heat Thermometer
graduated in Celsius degrees, having a range from 155 to
170°C and conforming to the requirements for Thermometer
1
This test method is under the jurisdiction of ASTM Committee D-8 on Roofing, 13C as prescribed in the Specification E 1.
Waterproofing, and Bituminous Materials and is the direct responsibility of 5.3 Container—The container in which the sample is to be
Subcommittee D08.03 on Surfacing and Bituminous Materials for Membrane
Waterproofing and Builtup Roofing. tested shall be of metal or glass, cylindrical in shape, and shall
Current edition approved Nov. 10, 1995. Published January 1996. Originally have a flat bottom. Its inside dimensions shall be substantially
published as D 6 – 10. Last previous edition D 6 – 80 (1990). as follows: diameter, 2.17 in. (55 mm), depth, 1.38 in. (35
2
Annual Book of ASTM Standards, Vol 04.03.
3
mm).
4
1
D6
Metric Equivalents
in. ⁄
1 16 ⁄
9 64 ⁄
14 ⁄
5 16 ⁄
23 64 15⁄32 1⁄2 3⁄4 115⁄32 11⁄2 215⁄16 47⁄8
mm 1.6 3.6 6.4 7.9 9.1 11.9 12.7 19.0 37.3 38.1 74.6 123.8
FIG. 1 Aluminum Shelf
NOTE 2—Containers known in the drug trade as seamless “ointment TABLE 1 Reproducibility of Results
boxes” may be obtained in dimensions conforming to the above require- Volatilization Loss, % Numerical Correction True Volatilization Loss, %
ments.
5.0 60.50 4.50 to 5.50
5.5 60.51 4.99 to 6.01
6. Technical Hazards 6.0 60.52 5.48 to 6.52
6.1 Under ordinary circumstances a number of samples 10.0 60.60 9.40 to 10.60
15.0 60.70 14.30 to 15.70
having about the same degree of volatility may be tested at the 25.0 60.90 24.10 to 25.90
same time. Samples varying greatly in volatility should be 40.0 61.20 38.80 to 41.20
tested separately. When extreme accuracy is required not more
than one material should be tested at one time and duplicate
samples of it should be placed simultaneously in the oven. that temperature. The 5-h period shall start when the tempera-
Such duplicates shall check within the limits of accuracy given ture reaches 324°F (162°C), and in no case shall the total time
in Section 9. Results obtained on samples showing evidences that a sample is in the oven be more than 5 h and 15 min. At
of foaming during the test shall be rejected. the conclusion of the heating period, remove the sample from
the oven, cool to room temperature, weigh to the nearest 0.01
7. Preparation of Sample
g, and calculate the loss due to heating.
7.1 Thoroughly stir and agitate the sample as received, 8.2 Determine temperatures by means of the specified
warming, if necessary, to obtain a complete mixture before the thermometer, which shall be supported from the shaft of the
portion for analysis is removed. circular shelf in a vertical position approximately 0.75 in. (19
7.2 First test the material under examination for water and, mm) inside the periphery of the shelf, and with the bottom of
if water is present, remove it by suitable methods of dehydra- the thermometer bulb 0.25 in. (6 mm) above the shelf.
tion before subjecting the material to the loss on heating test;
or, obtain another sample that is free of water. NOTE 3—If additional periods of heating are desired, it is recommended
that they be made in successive increments of 5 h each.
8. Procedure NOTE 4—When it is required that the penetration or other characteris-
8.1 Place 50.0 6 0.5 g of the sample of the water-free tics of the sample after heating be determined, the residue should be
melted in the container at the lowest possible temperature and thoroughly
material to be tested in a tared container conforming to the mixed by stirring, taking care to avoid incorporating air bubbles in the
requirements of 5.3, and weigh to the nearest 0.01 g. If the material. For the penetration test, the well-mixed residue shall be brought
material has been heated to facilitate transfer, cool the sample to standard temperature and tested as prescribed in Test Method D 5. For
to room temperature before making this initial weighing. Bring other tests, the well-mixed residue should be tested according to standard
the oven to a temperature of 325°F (163°C), and place the conditions as required by the test procedure involved.
container with the weighed sample on and near the circumfer-
ence of the circular shelf, in one of the recesses if the 9. Precision and Bias
recommended shelf is used. Close the oven and rotate the shelf 9.1 Up to 5 % loss in mass, the results obtained may be
during the entire test at a rate of 5 to 6 rpm. Maintain the considered as correct within 0.5. Above 5 % loss in mass, the
temperature at 325 6 1.8°F (163 6 1°C) for 5 h after the numerical limit of error increases 0.01 for every 0.5 % increase
sample has been introduced and the oven has again reached in loss by volatilization as shown in Table 1.
2
D6
9.2 Bias—The procedure in Test Method D 6 has no bias 10. Keywords
because the value of the loss on heating of oil and asphaltic
10.1 asphalt; heating; oil; oven
compounds test, is defined in terms of the test method.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428.

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Designation: D 6 – 95 American Association State

Highway and Transportation Officials Standard

Standard Test Method for

1. Scope (180°C). During the tests for compliance to Specification

FIG. 1 Aluminum Shelf

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