ASTM D6 D6M-1995(2011)e1 Standard Test Method for Loss on Heating of Oil and Asphaltic Compounds《油和柏油化合物加热减量用标准试验方法》.pdf

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1、Designation: D6/D6M 95 (Reapproved 2011)1American Association StateHighway and Transportation Officials StandardAASHTO No.: T47Standard Test Method forLoss on Heating of Oil and Asphaltic Compounds1This standard is issued under the fixed designation D6/D6M; the number immediately following the desig

2、nation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by

3、agencies of the Department of Defense.1NOTEUnits information was editorially revised in February 2011.1. Scope1.1 This test method covers the determination of the loss inmass (exclusive of water) of oil and asphaltic compounds whenheated as hereinafter prescribed.1.2 The values stated in either SI u

4、nits or inch-pound unitsare to be regarded separately as standard. The values stated ineach system may not be exact equivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems may result in non-conformancewith the standard.1.3 This standard does

5、not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility and regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Stand

6、ards:2D5 Test Method for Penetration of Bituminous MaterialsE1 Specification for ASTM Liquid-in-Glass ThermometersE145 Specification for Gravity-Convection and Forced-Ventilation Ovens3. Summary of Test Method3.1 Fifty grams of material, spread out in a dish 55 mm indiameter, is heated in moving air

7、 for 5 h at 163C 325F andthe percent loss of mass determined along with a comparison,before and after, of any other desired characteristics. This testmethod provides only a relative measurement of the volatilityof a material under test conditions.4. Significance and Use4.1 This test method is useful

8、 in characterizing certainpetroleum products by the determination of their loss of massupon heating under standardized conditions.5. Apparatus5.1 OvenThe oven shall be electrically heated and shallconform to the performance requirements of SpecificationE145 Type I, Grade B, for operating temperature

9、s up to 180C365F. During the tests for compliance to Specification E145requirements, the oven shelf, properly placed, shall be in placeand rotating. In addition, it shall also comply with thefollowing requirements:5.1.1 Construction (Note 1)The oven shall be rectangularwith minimum interior dimensio

10、ns of 330 mm 13 in. in eachdirection. The oven shall have in front a tightly fitting hingeddoor, which shall provide a clear opening substantially thesame as the interior height and width of the oven. The doormay contain a window with dimensions of at least 100 by 100mm 4 by 4 in., and with two shee

11、ts of glass separated by anair space, through which a vertical thermometer located asspecified in Section 8, may be read without opening the door;or the oven may be provided with an inner glass door, throughwhich the thermometer may be observed on opening the outerdoor momentarily. The oven shall be

12、 adequately ventilated byconvection currents of air and for this purpose shall beprovided with openings for the entrance of air and for the exitof heated air and vapors. Openings may be of any size andarrangement provided the requirements of Specification E145,Type I, Grade B, are met.5.1.2 Rotating

13、 ShelfThe oven shall be provided with acircular metal shelf having a minimum diameter of 250 mm9.8 in. (A recommended form of aluminum shelf is shown inFig. 1.) The shelf shall be suspended by a vertical shaft andcentered with respect to the horizontal interior dimensions. Theshelf shall be provided

14、 with a mechanical means of rotating it1This test method is under the jurisdiction ofASTM Committee D08 on Roofingand Waterproofing and is the direct responsibility of Subcommittee D08.03 onSurfacing and Bituminous Materials for Membrane Waterproofing and Built-upRoofing.Current edition approved Jan

15、. 1, 2011. Published February 2011. Originallyapproved in 1910. Last previous edition approved in 2006 as D6 95 (2006). DOI:10.1520/D0006_D0006M-95R11E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMS

16、tandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.at the rate of 5 to 6 rpm. The shelf shall be vertically locatedas close to the center of th

17、e oven as permitted by compliancewith the requirements of 7.2 regarding thermometer placement.NOTE 1Continued use of existing smaller ovens complying with therequirements of this test shall be permitted for an indefinite period toprovide for normal amortization of present equipment. However, all new

18、ovens purchased should comply with the minimum dimensions andrequirements of this test method.5.2 ThermometerAn ASTM Loss on Heat Thermometergraduated in Celsius degrees, having a range from 155 to170C and conforming to the requirements for Thermometer13C as prescribed in the Specification E1.5.3 Co

19、ntainerThe container in which the sample is to betested shall be of metal or glass, cylindrical in shape, and shallhave a flat bottom. Its inside dimensions shall be substantiallyas follows: diameter, 55 mm 2.17 in., depth, 35 mm 1.38in.NOTE 2Containers known in the drug trade as seamless “ointmentb

20、oxes” may be obtained in dimensions conforming to the above require-ments.6. Technical Hazards6.1 Under ordinary circumstances a number of sampleshaving about the same degree of volatility may be tested at thesame time. Samples varying greatly in volatility should betested separately. When extreme a

21、ccuracy is required not morethan one material should be tested at one time and duplicatesamples of it should be placed simultaneously in the oven.Such duplicates shall check within the limits of accuracy givenin Section 9. Results obtained on samples showing evidencesof foaming during the test shall

22、 be rejected.7. Preparation of Sample7.1 Thoroughly stir and agitate the sample as received,warming, if necessary, to obtain a complete mixture before theportion for analysis is removed.7.2 First test the material under examination for water and,if water is present, remove it by suitable methods of

23、dehydra-tion before subjecting the material to the loss on heating test;or, obtain another sample that is free of water.8. Procedure8.1 Place 50.0 6 0.5 g of the sample of the water-freematerial to be tested in a tared container conforming to therequirements of 5.3, and weigh to the nearest 0.01 g.

24、If thematerial has been heated to facilitate transfer, cool the sampleto room temperature before making this initial weighing. Bringthe oven to a temperature of 163C 325F, and place thecontainer with the weighed sample on and near the circumfer-ence of the circular shelf, in one of the recesses if t

25、herecommended shelf is used. Close the oven and rotate the shelfduring the entire test at a rate of 5 to 6 rpm. Maintain thetemperature at 163 6 1C 325 6 1.8F for 5 h after thesample has been introduced and the oven has again reachedthat temperature. The 5-h period shall start when the tempera-ture

26、reaches 162C 324F, and in no case shall the total timethat a sample is in the oven be more than 5 h and 15 min. Atthe conclusion of the heating period, remove the sample fromthe oven, cool to room temperature, weigh to the nearest 0.01g, and calculate the loss due to heating.8.2 Determine temperatur

27、es by means of the specifiedthermometer, which shall be supported from the shaft of theMetric Equivalentsin.mm1161.69643.6146.45167.923649.1153211.91212.73419.01153237.311238.12151674.6478123.8FIG. 1 Aluminum ShelfTABLE 1 Reproducibility of ResultsVolatilization Loss, % Numerical Correction True Vol

28、atilization Loss, %5.0 60.50 4.50 to 5.505.5 60.51 4.99 to 6.016.0 60.52 5.48 to 6.5210.0 60.60 9.40 to 10.6015.0 60.70 14.30 to 15.7025.0 60.90 24.10 to 25.9040.0 61.20 38.80 to 41.20D6/D6M 95 (2011)12circular shelf in a vertical position approximately 19 mm 0.75in. inside the periphery of the shel

29、f, and with the bottom of thethermometer bulb 6 mm 0.25 in. above the shelf.NOTE 3If additional periods of heating are desired, it is recommendedthat they be made in successive increments of 5 h each.NOTE 4When it is required that the penetration or other characteris-tics of the sample after heating

30、 be determined, the residue should bemelted in the container at the lowest possible temperature and thoroughlymixed by stirring, taking care to avoid incorporating air bubbles in thematerial. For the penetration test, the well-mixed residue shall be broughtto standard temperature and tested as presc

31、ribed in Test Method D5. Forother tests, the well-mixed residue should be tested according to standardconditions as required by the test procedure involved.9. Precision and Bias9.1 Up to 5 % loss in mass, the results obtained may beconsidered as correct within 0.5. Above 5 % loss in mass, thenumeric

32、al limit of error increases 0.01 for every 0.5 % increasein loss by volatilization as shown in Table 1.9.2 BiasThe procedure in Test Method D6 has no biasbecause the value of the loss on heating of oil and asphalticcompounds test, is defined in terms of the test method.10. Keywords10.1 asphalt; heat

33、ing; oil; ovenASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of su

34、ch 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 andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for addi

35、tional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to th

36、e ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D6/D6M 95 (2011)13