1、Designation: D 36 06Standard Test Method forSoftening Point of Bitumen (Ring-and-Ball Apparatus)1This standard is issued under the fixed designation D 36; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision.An
2、umber in parentheses indicates the year of last reapproval.Asuperscriptepsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers the determination of the soft-en
3、ing point of bitumen in the range from 30 to 157C (86 to315F) using the ring-and-ball apparatus immersed in distilledwater (30 to 80C), USP glycerin (above 80 to 157C), orethylene glycol (30 to 110C).1.2 The values stated in SI units are to be regarded as thestandard.1.3 This standard does not purpo
4、rt 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 of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C 67
5、0 Practice for Preparing Precision and Bias Statementsfor Test Methods for Construction MaterialsD92 Test Method for Flash and Fire Points by ClevelandOpen Cup TesterD 140 Practice for Sampling Bituminous MaterialsD 3461 Test Method for Softening Point of Asphalt andPitch (Mettler Cup-and-Ball Metho
6、d)E1 Specification for ASTM Liquid-in-Glass Thermometers3. Summary of Test Method3.1 Two horizontal disks of bitumen, cast in shoulderedbrass rings, are heated at a controlled rate in a liquid bath whileeach supports a steel ball. The softening point is reported as themean of the temperatures at whi
7、ch the two disks soften enoughto allow each ball, enveloped in bitumen, to fall a distance of25 mm (1.0 in.).4. Significance and Use4.1 Bitumens are viscoelastic materials without sharplydefined melting points; they gradually become softer and lessviscous as the temperature rises. For this reason, s
8、ofteningpoints must be determined by an arbitrary and closely definedmethod if results are to be reproducible.4.2 The softening point is useful in the classification ofbitumens, as one element in establishing the uniformity ofshipments or sources of supply, and is indicative of thetendency of the ma
9、terial to flow at elevated temperaturesencountered in service.5. Apparatus5.1 RingsTwo square-shouldered brass rings conformingto the dimensions shown in Fig. 1(a).5.2 Pouring Plate A flat, smooth, brass plate approxi-mately 50 by 75 mm (2 by 3 in.).5.3 BallsTwo steel balls, 9.5 mm (38 in.) in diame
10、ter, eachhaving a mass of 3.50 6 0.05 g.5.4 Ball-Centering GuidesTwo brass guides for centeringthe steel balls, one for each ring, conforming to the generalshape and dimensions shown in Fig. 1 (b).5.5 BathA glass vessel, capable of being heated, not lessthan 85 mm in inside diameter and not less tha
11、n 120 mm indepth from the bottom of the flare.NOTE 1An 800-mL, low-form Griffin beaker of heat-resistant glassmeets this requirement.5.6 Ring Holder and AssemblyA brass holder designed tosupport the two rings in a horizontal position, conforming tothe shape and dimensions shown in Fig. 1 (c), suppor
12、ted in theassembly illustrated in Fig. 1 (d). The bottom of the shoulderedrings in the ring holder shall be 25 mm (1.0 in.) above theupper surface of the bottom plate, and the lower surface of thebottom plate shall be 16 6 3mm(58 618 in.) from the bottomof the bath.5.7 Thermometers:5.7.1 An ASTM Low
13、 Softening Point Thermometer, havinga range from 2 to + 80C or 30 to 180F, and conforming tothe requirements for Thermometer 15C or 15F as prescribed inSpecification E1. As an alternative, any other thermometricdevice used shall be at least: (1) of equal accuracy to that of the1This test method is u
14、nder 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 Dec. 1, 2006. Published December 2006. Originallyapproved in 196
15、2. Last previous edition approved in 2000 as D 36 95 (2000)e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website
16、.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.thermometer specified in Specification E1,(2) capable ofindicating temperature to within 1C (2F), and (3) stable towithin 1C (2F) for the duration of the exposure.5.7.2 AnASTM High Sof
17、tening Point Thermometer, havinga range from 30 to 200C or 85 to 392F, and conforming to therequirements for Thermometer 16C or 16F as prescribed inSpecification E1. As an alternative, any other thermometricdevice used shall be at least: (1) of equal accuracy to that of thethermometer specified in S
18、pecification E1,(2) capable ofindicating temperature to within 1C (2F), and (3) stable towithin 1C (2F) for the duration of the exposure.5.7.3 The appropriate thermometer shall be suspended inthe assembly as shown in Fig. 1 (d) so that the bottom of thebulb is level with the bottom of the rings and
19、within 13 mm(0.5 in.) of the rings, but not touching them or the ring holder.Substitution of other thermometers shall not be permitted. Asan alternative, any other thermometric device used shall be atleast: (1) of equal accuracy to that of the thermometer specifiedin Specification E1,(2) capable of
20、indicating temperature towithin 0.5C (1.0F), and (3) stable to within 0.5C (1.0F) forthe duration of the exposure.6. Reagents and Materials6.1 Bath Liquids:6.1.1 Freshly Boiled Distilled Water.NOTE 2The use of freshly boiled distilled water is essential to avoidtrapping air bubbles on the surface of
21、 the specimen which may affect theresults.6.1.2 USP Glycerin (WarningGlycerin has a flash pointof 160C (320F) in accordance with Test Method D92.), or6.1.3 Ethylene Glycol, with a boiling point between 195 and197C (383 and 387F). (WarningEthylene glycol is toxicwhen taken internally or inhaled as a
22、vapor.Avoid prolonged orrepeated skin contact and inhalation of vapors. Its flash point is115C (239F) in accordance with Test Method D92. Whenusing this bath liquid, conduct the test in a vented laboratoryhood with adequate exhaust fan capacity to ensure removal oftoxic vapors.)6.2 Release Agents:6.
23、2.1 To prevent adhesion of bitumen to the pouring platewhen casting disks, the surface of the brass pouring plate maybe thinly coated just before use with silicone oil or grease, aNOTE 1All dimensions are in millimetres.FIG. 1 Shouldered Ring, Ball-Centering Guide, Ring Holder, and Assembly of Appar
24、atus Showing Two RingsD36062mixture of glycerin and dextrin, talc, or china clay.(WarningIsolate silicones from other bituminous testingequipment and samples to avoid contamination, and weardisposable rubber gloves whenever handling silicones or ap-paratus coated with them. Silicone contamination ca
25、n produceerroneous results in other tests such as those for penetrationand flash point.)7. Sampling7.1 Sample the material in accordance with Practice D 140.8. Test Specimens8.1 Do not start unless it is planned to complete preparationand testing of all asphalt specimens within 6 h and all coal-tarp
26、itch specimens within 412 h. Heat the bitumen sample withcare, stirring frequently to prevent local overheating, until ithas become sufficiently fluid to pour (Note 3). Stir carefully toavoid incorporation of air bubbles in the sample.NOTE 3An electric hot plate having a minimum power to unit-surfac
27、e-area ratio of 37 kW/m2has been found satisfactory for thispurpose.8.1.1 Take no more than2htoheat an asphalt sample to itspouring temperature; in no case shall this be more than 110C(200F) above the expected softening point of the asphalt.8.1.2 Take no more than 30 min to heat a coal-tar pitchsamp
28、le to its pouring temperature; in no case shall this be morethan 55C (100F) above the expected softening point of thecoal-tar-pitch.8.1.3 If the test must be repeated later, do not reheat thissample; use a fresh sample in a clean container to prepare newtest specimens.8.2 Heat the two brass rings (b
29、ut not the pouring plate) tothe approximate pouring temperature, and place them on thepouring plate treated with one of the release agents.8.3 Pour a slight excess of the heated bitumen into eachring, and then allow the specimens to cool in ambient air for atleast 30 min. For materials that are soft
30、 at room temperature,cool the specimens for at least 30 min at an air temperature atleast 10C (18F) below the expected softening point. From thetime the specimen disks are poured, no more than 240 minshall elapse before completion of the test.8.4 When the specimens have cooled, cut away the excessbi
31、tumen cleanly with a slightly heated knife or spatula, so thateach disk is flush and level with the top of its ring.9. Procedure9.1 Select one of the following bath liquids and thermom-eters appropriate for the expected softening point:9.1.1 Freshly boiled distilled water for softening pointsbetween
32、 30 and 80C (86 and 176F); use Thermometer 15C or15F. The starting bath temperature shall be 5 61C (41 6 2F).9.1.2 USP glycerin for softening points above 80C (176F)and up to 157C (315F); use Thermometer 16C or 16F. Thestarting bath temperature shall be 30 6 1C (86 6 2F).9.1.3 Ethylene glycol for so
33、ftening points between 30 and110C (86 and 230F); use Thermometer 16C or 16F. Thestarting bath temperature shall be 5 6 1C (41 6 2F).9.1.4 For referee purposes, all softening points up to 80C(176F) shall be determined in a water bath and all softeningpoints above 80C (176F) shall be determined in a g
34、lycerinbath.9.2 Assemble the apparatus in the laboratory hood with thespecimen rings, ball-centering guides, and thermometer inposition, and fill the bath so that the liquid depth will be 105 63mm(418 618 in.) with the apparatus in place. If usingethylene glycol, make sure the hood exhaust fan is tu
35、rned onand operating properly to remove toxic vapors. Using forceps,place the two steel balls in the bottom of the bath so they willreach the same starting temperature as the rest of the assembly.9.3 Place the bath in ice water, if necessary, or gently heat toestablish and maintain the proper starti
36、ng bath temperature for15 min with the apparatus in place. Take care not to contami-nate the bath liquid.9.4 Again using forceps, place a ball from the bottom of thebath in each ball-centering guide.9.5 Heat the bath from below so that the temperatureindicated by the thermometer rises at a uniform r
37、ate of 5C(9F)/min (Note 4). Protect the bath from drafts, using shieldsif necessary. Do not average the rate of temperature rise overthe test period. The maximum permissible variation for any1-min period after the first 3 min shall be 60.5C (61.0F).Reject any test in which the rate of temperature ri
38、se does notfall within these limits.NOTE 4Rigid adherence to the prescribed heating rate is essential toreproducibility of results. Either a gas burner or electric heater may beused, but the latter must be of the low-lag, variable output type to maintainthe prescribed rate of heating.9.6 Record for
39、each ring and ball the temperature indicatedby the thermometer at the instant the bitumen surrounding theball touches the bottom plate. Make no correction for theemergent stem of the thermometer. If the difference betweenthe two temperatures exceeds 1C (2F), repeat the test.10. Calculation10.1 For a
40、 given bitumen specimen, the softening pointdetermined in a water bath will be lower than that determinedin a glycerin bath. Since the softening point determination isnecessarily arbitrary, this difference matters only for softeningpoints slightly above 80C (176F).10.2 The change from water to glyce
41、rin for softening pointsabove 80C creates a discontinuity. With rounding, the lowestpossible asphalt softening point reported in glycerin is 84.5C(184F), and the lowest possible coal-tar pitch softening pointreported in glycerin is 82.0C (180F). Softening points inglycerin lower than these translate
42、 to softening points in waterof 80C (176F) or less, and shall be so reported.10.2.1 The correction for asphalt is 4.2C (7.6F), andfor coal-tar pitch is 1.7C (3.0F). For referee purposes,repeat the test in a water bath.10.2.2 Under any circumstances, if the mean of the twotemperatures determined in g
43、lycerin is 80.0C (176.0F) orlower for asphalt, or 77.5C (171.5F) or lower for coal-tarpitch, repeat the test in a water bath.10.3 To convert softening points slightly above 80C(176F) determined in water to those determined in glycerin,D36063the correction for asphalt is + 4.2C ( + 7.6F) and for coal
44、-tarpitch is + 1.7C ( + 3.0F). For referee purposes, repeat the testin a glycerin bath.10.3.1 Under any circumstances, if the mean of the twotemperatures determined in water is 85.0C (185.0F) orhigher, repeat the test in a glycerin bath.10.4 Results obtained by using an ethylene glycol bath willvary
45、 from those using water and glycerin. The followingformulas shall be used to calculate the differences:Asphalt:SP glycerin! 5 1.026 583 3 SP ethylene glycol! 2 1.334 968C(1)SP water! 5 0.974 118 3 SP ethylene glycol! 2 1.444 59C(2)Coal Tar:SP glycerin! 5 1.044 795 3 SP ethylene glycol! 2 5.063 574C(
46、3)SP water! 5 1.061 111 3 SP ethylene glycol! 2 8.413 488C(4) Editorially corrected.11. Report11.1 When usingASTM Thermometer 15C or 15F, report tothe nearest 0.2C or 0.5F the mean or corrected mean of thetemperatures recorded in 9.6 as the softening point.11.2 When using ASTM Thermometer 16C or 16F
47、 report tothe nearest 0.5C or 1.0F the mean or corrected mean of thetemperatures recorded in 9.6 as the softening point.11.3 Report the bath liquid used in the test.12. Precision and Bias12.1 With distilled water or USP glycerin, the followingcriteria shall be used for judging the acceptability of r
48、esults(95 % probability):12.1.1 Single-Operator PrecisionThe single-operatorstandard deviation has been found to be 0.41C (0.73F).Therefore, results of two properly conducted tests by the sameoperator on the same sample of bitumen should not differ bymore than 1.2C (2.0F).312.1.2 Multilaboratory Pre
49、cisionThe multilaboratorystandard deviation has been found to be 0.70C (1.26F).Therefore, results of two properly conducted tests on the samesample of bitumen from two laboratories should not differ bymore than 2.0C (3.5F).312.2 With ethylene glycol, the following criteria shall beused for judging the acceptability of results:12.2.1 Single-Operator PrecisionThe single-operatorstandard deviation has been found to be 0.72C (1.29F).Therefore, res
