tae Standard Specification for Loss on Heating of Oil and Asphaltic Compounds AASHTO DESIGNATION: T 47-83 (1996) AASHTO T 47-83 (1996) is identical to ASTM D 6-80 (1990) except that Section 6.1 of ASTM D 6-80 (1990) shall be replaced with the following: 6.1 Heat the sample with care, string as necessary, to prevent local overheating until it has become sufficiently fluid to pour. In a0 case should the temperature be raised to more than 100°C or 180°F above the expected softening point. 68-= TAT qq) Designation: D 6 ~ 80 (Reapproved 1990) Standard Test Method for METHODS OF SAMPLING AND TESTING Cc _Aercan sass Sain Highway ana Tarapotaten ORs Sasso ASTON TT Loss on Heating of Oil and Asphaltic Compounds’ “his standard sand ender the ied dsgntion D 6; the number immediately flowing the decignation indicts the year of oreinal adoption rin the case of revision, the year fast revi. A number in parentheses indicates the yea fast eappeval A sopenrpt elon (indicates an editonal change since the last revision ot approval 1. Scope 1.1 This test method covers the determination of the loss in mass (exclusive of water) of oll and asphaltic compounds when heated as hereinafter prescribed. 1.2 The values in inch-pound units are to be regarded as standard. The values in parentheses are for information only 1.3 This standard does not purport to address all of the safety problems associated with its use. Iti the responsibility ofthe user ofthis standard to establish appropriate safety and health practices and determine the applicability and regula tory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D3 Test Method for Penetration of Bituminous Materials? E | Specification for ASTM Thermometers? E 145 Specification for Gravity-Convection: and Forced- ‘Ventilation Ovens* 3. Summary of Test Method 3.1. Fifty grams of material, spread out in a dish $3 mm in iameter, is heated in moving air for 5 h at 325°F (163°C) and the percent loss of mass determined along with a comparison, before and after, of any other desired character- istics. This test method provides only a relative measurement of the volatility of a material under test conditions. 4. Apparatus 4.1 Oven—The oven shall be electrically heated and shall conform to the performance requirements of Specification E145 Type 1, Grade B, for operating temperatures up 10 365°F (180°C), During the tests for compliance to Specifica- tion E 145 requirements, the oven shelf, properly placed shall be in place and rotating. In addition, it shall also comply with the following requirements: 4.1.1 Construction (Note 1)—The oven shall be rectan- gular with minimum interior dimensions of 13 in. (330 mm) in each direction. The oven shall have in front a tightly fiting hinged door, which shall provide a clear opening substantially the same as the interior height and width of the oven, The door may contain a window with dimensions of at least 4 by in, (100 by 100 mm), and with two sheets of glass "This test method is under the jursicuon of ASTM Commitee 0-8 on Roofing. Watereroting, and Bituminous Materals ad she vec response ¥ Subcommitee 08.03 Surtfaang ana Drone Matera fr Merman Wateometing sre Bul 7 ‘Caren editon approved May 30, 1980, Published Jay 1980. Orignaly Dubished ac D'6" 10 Lat previous eon D6 671973) ® tna Book of ASTM Standard, Vol 0408, mn Boos of ASTM Standards, Vols 08.03 and 1203. “nual Book of ASTM Standards Vol 1402 separated by an air space, through which a vertical thermom- eter located as specified in Section 7, may be read without ‘opening the door; or the oven may be provided with an inner lass door, through which the thermometer may be observed on opening the outer door momentarily. The oven shall be adequately ventilated by convection currents of air and for this purpose shall be provided with openings for the entrance of air and for the exit of heated air and vapors. Openings ‘may be of any size and arrangement provided the require- ‘ments of Specification E 145, Type 1, Grade B, are met. 4.1.2 Rotating Shelf—The oven shall be provided with a circular metal shelf having a minimum diameter of 9.8 in. (250 mm). (A recommended form of aluminum shelf is shown in Fig. 1.) The shelf shall be suspended by a vertical shaft. and centered with respect to the horizontal interior dimensions. The shelf shall be provided with a mechanical ‘means of rotating it at the rate of 5 to 6 rpm. The shelf shall be vertically located as close to the center of the oven as permitted by compliance with the requirements of 6.2 Tegarding thermometer placement. Nore 1—Continued use of existing smaller ovens complying with the requirements ofthis test shall be permitted fr an indefinite period to provige for normal amortization of present equipment. However all ‘Rew ovens purchased should comply withthe minimum dimensions and requirements ofthis test method. 4.2 Thermometer—An ASTM Loss on Heat Thermom- ter graduated in Celsius degrees, having a range from 155 10 170°C and conforming to the requirements for Thermometer 13C as prescribed in the Specification E 1 4.3 Container—The container in which the sample is to be tested shall be of metal or glass, cylindrical in shape, and shall have a flat bottom, Its inside dimensions shall be substantially as follows: diameter, 2.17 in. (55 mm), depth, 1,38 in. (35 mm). Nore 2—Containers known in the drug trade a8 seamless “ointment bores” may be obtained in dimensions conformine 40 the above requirements, 5. Technical Hazards 5.1 Under ordinary circumstances a number of samples having about the same degree of volatility may be tested at the same time. Samples varying greatly in volatility should be 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. Such duplicates shall check within the limits of accuracy given in Section 8. Results obtained on samples showing evidences of foaming during the test shall be rejected, 6. Preparation of Sample 6.1 Thoroughly stir and agitate the sample as received,0 METHODS OF SAMPLING AND TESTING Ta qb vs oe ph Gee we Section A-B Metic Equivaients ee % we Ree % % Te 7 Dh ee mt 36 sk 78a HD FIG. 1 Aluminum Shelf wars, if necessary, 10 ensure a complete mixture before the poctioa for analysis is removed. 6.2 First test the material under examination for water aad, it yaicr is present, remove it by suitable methods of dehyleation before subjecting the material to the loss on * hoating test; o¢, obtain another sample that is free of water, 7. Procedure 7.1 Place 50.0 £ 0.5 g of the sample of the water-free ‘material to be tested in a tared container conforming to the requirements of 4.3, and weigh to the nearest 0.01 g. If the material has been ‘heated to facilitate transfer, cool the sample to room temperature before making this initial weighing, Dring the oven to a temperature of 325°F (163°C), and vlncs the container with the weighed sample on and near the ciscumference of the circular shelf, in one of the recesses if the recommended shelf is used. Close the oven and rotate the shelf during the entire test at a rate of 5 to 6 rpm. Maintain the temperature at 325 + 1.8°F (163 + 1°C) for Sh after the sample has been introduced and the oven has again reached that temperature. The 5-h period shall start when the temperature reaches 324°F (162°C), and in no case shall the total time that a sample is in the oven be more than 5h and 15 min, At the conclusion of the heating period, remove the sample from the oven, cool to room temperature, weigh to the nearest 0.01 g, and calculate the loss due to heating. 7.2. Determine temperatures by means of the specified thermometer, which shall be supported from the shaft of the circular shelf in a vertical position approximately 0.75 in. (19 mm) inside the periphery of the shelf, and with the bottom of the thermometer bulb 0.25 in. (6 mm) above the shelf. Nore 3—If additional periods of heating are desired, itis recom- ‘mended that they be made in successive increments of $b each. ‘Nore 4—When its required thatthe penetration or other character istics of the sample after heating be determined, the residue should be melted in the container atthe lovest possible temperature and thor- ‘oughly mixed by string, taking care to avoid incorporating air bubbles in the material For the penetration test, the well-mixed residve shall be Drought to standard temperature and tested as prescribed in Test ‘Method D 5. For other tests, the well-mixed residue should be tested ‘according to standard conditions as required by the test procedure involved, 8, Reproducibility of Results 8.1 Up to 5% loss in mass, the results obtained may be considered as correct within 0.5. Above 5 % loss in mass, the ‘numerical limit of error increases 0.01 for every 0.5 % increase in loss by volatilization as shown in Table 1. TABLE 1 Reproducioility of Results ‘Woatlaaton Loss, Numerical Corecton —Trve Vola 30 050 “450 10 550 55 #051 49910601 60 #052 5.8 to 652 100 20.60 98.40 1010.60 380 070 142910 1570 250 090 2430102590 400 3120, 38.80 1041.20 1 ‘The American Society for Testing and Maal tkes no postion respecting the vay o any pate rights assorted in conection wth any ken mortoned inthis stancard. Users a this Sanaa’ are exrassy advised that etermnaion othe vay of ay such alot rigs, and the rk of irtingement of such rights, ae eta the own responsi. Vows inown foe ASTI Commitee on Sandards, 1916 Race St, Padi, PA 18102,