ip Designation: D 6 - 80 (Reapproved 1990) Standard Test Method for Loss on Heating of Oi! and Asphal “This sander issued under the gina asontion othe pmccan Assocaton Site Horny na aneporaton Ga Stra Compounds* ‘ed designation Dé: the umber immedatl following the designation indicates the year of sof ron the ver of eon, A Bombe npareatheses indicates the ver ofa approval. A Sipeteap sss (indiates av editors shange ence ne ast reision Or Texpproval 1. Scope 1.1 This test method covers the determination of the loss, in mass (exclusive of water) of oil and asphaltic compounds after prescribed, n inch-pound units are to be regarded as 25 are for information only is standard does nor purpar: 10 address all a the sajery problems associated with its use. 1 isthe responsibility of the user of this standard to establish appropriate safety and hhealth practices and devermiine the applicability and regula: tory limitations prior 10 use. 2. Referenced Documents 241 ASTM Standards: DS Test Method for Penetration of Bituminous Materials* E | Specification for ASTM Thermometers E 148 Specification for Gravity-Convection and Forced- Ventilation Ovens 3. Summary of Test Method 3.1. Fifty grams of material. spread out in a dish $5 mm in iameter, is heated in moving air for $ h at 325°F (163°C) and the percent loss of mass determined along with @ ‘comparison, before and after, of any other desired characte 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 clectrcally 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 (Nove I}—The oven shall be rectan gular with minimum interior dimensions of (3 in. (330 mm) in cach direction. The oven shall have in front 2 tightly fitting 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 Teast 4 by 4 in. (100 by 100 mm). and with two sheets of lass, ‘This tet methos f under enc suntaicuan of ASTM Commies DS on Roofing, Watermain ans Bxuminous Matenale anc he sent espns ff Subeommiter DUE 03 on Surfazng ane Brumious Mate fo: Membrane Waterproofing ane Boer Rooting Caner eon pubieres 9 DE fnaua’ Boo Pasisned Ju 1980. Onin separated by an airspace. through which e vertical thermom:- ater located as specified in Section 7. may be read without opening the door: or the oven may be provided with an inner glass door. through which the thermometer may be observed fon opening the outer door momentarily. The oven shall be adequately ventilated by convection currents of air an for this purpose shall be provided with openings for the entrance Of air and for the exit of heated air and vapors. Openings mas be of any size and arrangement provided the require- rents of Specification E 145, Type 1. Grade B, are m: ‘41.2 Rotating Shel/—The oven shall be provided with 2 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 reans of rotating it atthe rate of Sto 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 regarding thermometer placement. Nore 1—Comsinued use of existing smaller ovens complying with the recuirements of this est shal be permitted for an edefine penoe 1 provide for normal amorization of present equipment. Ho ew ovens purchased should comply wit the minimum dimension and requirement ft test method 4.2 Thermometer—An ASTM Loss on Heat Thermom- ‘ver graduated in Celsius degrees, having a range from 155 to 170°C and conforming to the requirements for Thermometer 13C as prescribed in the Specification E 1 43 Container—The container in which the sample is to 32 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 ja. (35 mm). Nore 2—Contaners known i the drug wade as seamless "oinment boses” may be obtained in dimensions conforming to the above seouiements 5. Technical Hazards $1 Under ordinary circumstances a number of samples having about the same degree of volatility may be teste 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 sampies showing evidences of foaming during the test shall be rejected 6. Preparation of Sample 6.1 Thoroughly stir and agitate the sample as received, th2 tsond is a em Bs be Fis. 1 warming, if necessary. 10 ensure a complete mixture before the portion for analysis is removed. 6.2 First test the material under examination for water and, if water is present, remove it by suitable methods of dehydration before subjecting the material to the loss on heating test: of. obtain another sample that is free of water 7. Procedure 7.1 Place 30.0 = 0.5 g of the sample of the watersiree 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 10 facilitate transfer. cool the sample to room temperature before making this inital ‘weighing. Bring the oven to a temperature of 325°F (163"C). and place the container withthe weighed sample on and near the circumference of the circular shel. 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 mpm Maintain the temperature at 325 + L.8°F (163+ °C) for Sh ater the sample has been introduced and the oven fas again reached that temperature, The S-h period shall start when the temperature reaches 324°F (162°C), and in ao case shall the total time that a sample is in the oven be mere than $ h and 15 min, At the conclusion ofthe heating period, remove the sample from the oven, cool 10 room temperature. weigh to the nearest 0.01 g. and calculate the loss due to heatin 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 ‘Tne Amancan Soeay fr Testing and Matenals kas no postion aspect the acy of any sate ints asec 7 Te tae oa at ewe Alumiqum Shett ‘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 desied. itis ecom- mended that they be made in successive increments of 5h each ‘Note 4—When itis required that the penetration or other character. istics of the sample afer heating be determined. the residue should be ‘melted in the container at the lowest posible temperature and thor Dughly mixed 5» surnag. taking care to avoid incorporating air bubbles inthe materia, For the penetration test. the wellmised residue shall be brought 10 standard temperature and tested as presenbed ia. Test Method DS. For other tsi. the well-mined residue should be tested according (© 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 | TABLE 1 Reproducibility of Results 548 108.52 320010 33093 3880.0 41.20 280 400 wih ary tem manfaned inh saraar. Users of his andard are sxressy 20Wsed tal deena of e vay ot any Suen ‘ate ght, and the nek of itangemen of sven gs. ae reel Mar OW” respons. “Thi standard sujet fo revi at any tne bythe sparse ecnncal commie and must be reviewed every ve years anc toot reed, eer reaporoved or rcrawn, Your cone afe ite athe! for ensicn oh stance seater sane ‘ang seul be eocrsaed fo ASTM Howdarer, Your comments wil rcaive cal canseraton at 2 meting of he response ‘echnical commites, whch you nay ate It you te! hat your comments have ne ecaves 2 Tae Peaing yOu shoul mae your ‘tows town a the ASTM Commitee on Stndarae, 1976 Race St. Pmiageena, PA 19103