1、Designation: D36/D36M 09Standard Test Method forSoftening Point of Bitumen (Ring-and-Ball Apparatus)1This standard is issued under the fixed designation D36/D36M; the number immediately following the designation indicates the yearof original adoption or, in the case of revision, the year of last rev
2、ision. A number in parentheses indicates the year of last reapproval.A superscript epsilon () 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
3、the soft-ening point of bitumen in the range from 30 to 157C 86 to315F using the ring-and-ball apparatus immersed in distilledwater 30 to 80C or USP glycerin (above 80 to 157C).1.2 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard. The values stated in
4、each 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 not purport to address all of thesafety concerns, if any, associated with its use. It i
5、s 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:2C670 Practice for Preparing Precision and Bias Statementsfor Test Methods for Cons
6、truction MaterialsD92 Test Method for Flash and Fire Points by ClevelandOpen Cup TesterD140 Practice for Sampling Bituminous MaterialsD3461 Test Method for Softening Point of Asphalt andPitch (Mettler Cup-and-Ball Method)E1 Specification for ASTM Liquid-in-Glass Thermometers3. Summary of Test Method
7、3.1 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 which the two disks soften enoughto allow each ball, enveloped in bitumen, to fall a
8、 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, softeningpoints must be determined by an arbitrary and closely definedmethod if resul
9、ts 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 material to flow at elevated temperaturesencountered in service.5. Apparatus5.1 RingsT
10、wo square-shouldered brass rings conformingto the dimensions shown in Fig. 1(a).5.2 Pouring PlateA 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 diameter, eachhaving a mass of 3.50 6 0.05 g.5.4 Ball-Centering GuidesTwo brass guides for cent
11、eringthe 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 than 120 mm indepth from the bottom of the flare.NOTE 1An 800-mL, low-form Griffin beaker of
12、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), supported in theassembly illustrated in Fig. 1 (d). The bottom of the shoulderedrings in the rin
13、g 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 3mm58 618 in. from the bottomof the bath.5.7 Thermometers:5.7.1 An ASTM Low Softening Point Thermometer, havinga range from 2 to + 80C or 30 to 180F, and conforming to1T
14、his 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 Dec. 15, 2009. Published January 2010. Origi
15、nallyapproved in 1962. Last previous edition approved in 2006 as D36 06. DOI:10.1520/D0036_D0036M-09.2For 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 D
16、ocument Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.the requirements for Thermometer 15C or 15F as prescribed inSpecification E1. As an alternative, any other thermometricdevice used shall be at le
17、ast: (1) of equal accuracy to that of thethermometer 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 Softening Point Thermometer, havinga range from 30 to 200C or 85 to 392F, and conf
18、orming 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 Specification E1,(2) capable ofindicating temperature to within 1C 2F, and (3) s
19、table 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 within 13 mm0.5 in. of the rings, but not touching them or the ring holder.Substitu
20、tion 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 indicating temperature towithin 0.5C 1.0F, and (3) stable to within 0.5C 1.0F forthe
21、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 the specimen which may affect theresults.6.1.2 USP Glycerin.(WarningGlycerin has a flash
22、 pointof 160C 320F in accordance with Test Method D92.)6.2 Release Agents:6.2.1 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, amixture of glycerin and dextrin, talc, or ch
23、ina clay.(WarningIsolate silicones from other bituminous testingNOTE 1All dimensions are in millimetres (60.3 mm except where noted).FIG. 1 Shouldered Ring, Ball-Centering Guide, Ring Holder, and Assembly of Apparatus Showing Two RingsD36/D36M 092equipment and samples to avoid contamination, and wea
24、rdisposable rubber gloves whenever handling silicones or ap-paratus coated with them. Silicone contamination can produceerroneous results in other tests such as those for penetrationand flash point.)7. Hazards7.1 WarningMercury has been designated by EPA andmany state agencies as a hazardous materia
25、l that can causecentral nervous system, kidney, and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EP
26、As website,http:/www.epa.gov/mercury/faq.htm, for additional informa-tion. Users should be aware that selling mercury and/ormercury containing products into your state may be prohibitedby state law.8. Sampling8.1 Sample the material in accordance with Practice D140.9. Test Specimens9.1 Do not start
27、unless it is planned to complete preparationand testing of all asphalt specimens within 6 h and all coal-tarpitch 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
28、 incorporation of air bubbles in the sample.NOTE 3An electric hot plate having a minimum power to unit-surface-area ratio of 37 kW/m2has been found satisfactory for thispurpose.9.1.1 Take no more than2htoheat an asphalt sample to itspouring temperature; in no case shall this be more than 110C200F ab
29、ove the expected softening point of the asphalt.9.1.2 Take no more than 30 min to heat a coal-tar pitchsample to its pouring temperature; in no case shall this be morethan 55C 100F above the expected softening point of thecoal-tar-pitch.9.1.3 If the test must be repeated later, do not reheat thissam
30、ple; use a fresh sample in a clean container to prepare newtest specimens.9.2 Heat the two brass rings (but not the pouring plate) tothe approximate pouring temperature, and place them on thepouring plate treated with one of the release agents.9.3 Pour a slight excess of the heated bitumen into each
31、ring, and then allow the specimens to cool in ambient air for atleast 30 min. For materials that are soft 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
32、minshall elapse before completion of the test.9.4 When the specimens have cooled, cut away the excessbitumen cleanly with a slightly heated knife or spatula, so thateach disk is flush and level with the top of its ring.10. Procedure10.1 Select one of the following bath liquids and thermom-eters appr
33、opriate for the expected softening point:10.1.1 Freshly boiled distilled water for softening pointsbetween 30 and 80C 86 and 176F; use Thermometer 15C or15F. The starting bath temperature shall be 5 61C 41 6 2F.10.1.2 USP glycerin for softening points above 80C176F and up to 157C 315F; use Thermomet
34、er 16C or16F. The starting bath temperature shall be 30 6 1C 86 62F.10.1.3 For referee purposes, all softening points up to 80C176F shall be determined in a water bath and all softeningpoints above 80C 176F shall be determined in a glycerinbath or as agreed to by seller and buyer.10.2 Assemble the a
35、pparatus 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 63mm418 618 in. with the apparatus in place. Using forceps,place the two steel balls in the bottom of the bath so they willreach the same
36、starting temperature as the rest of the assembly.10.3 Place the bath in ice water, if necessary, or gently heatto establish and maintain the proper starting bath temperaturefor 15 min with the apparatus in place. Take care not tocontaminate the bath liquid.10.4 Again using forceps, place a ball from
37、 the bottom ofthe bath in each ball-centering guide.10.5 Heat the bath from below so that the temperatureindicated by the thermometer rises at a uniform rate of 5C9F/min (Note 4). Protect the bath from drafts, using shieldsif necessary. Do not average the rate of temperature rise overthe test period
38、. 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 rise does notfall within these limits.NOTE 4Rigid adherence to the prescribed heating rate is essential toreproducibility of results. Either a gas burne
39、r or electric heater may beused, but the latter must be of the low-lag, variable output type to maintainthe prescribed rate of heating.10.6 Record for each ring and ball the temperature indicatedby the thermometer at the instant the bitumen surrounding theball touches the bottom plate. Make no corre
40、ction for theemergent stem of the thermometer. If the difference betweenthe two temperatures exceeds 1C 2F, repeat the test.11. Calculation11.1 For a given bitumen specimen, the softening pointdetermined in a water bath will be lower than that determinedin a glycerin bath. Since the softening point
41、determination isnecessarily arbitrary, this difference matters only for softeningpoints slightly above 80C 176F.11.2 The change from water to glycerin for softening pointsabove 80C creates a discontinuity. With rounding, the lowestpossible asphalt softening point reported in glycerin is 84.5C184F, a
42、nd the lowest possible coal-tar pitch softening pointreported in glycerin is 82.0C 180F. Softening points inglycerin lower than these translate to softening points in waterof 80C 176F or less, and shall be so reported.11.2.1 The correction for asphalt is 4.2C 7.6F, andfor coal-tar pitch is 1.7C 3.0F
43、. For referee purposes,repeat the test in a water bath.D36/D36M 09311.2.2 Under any circumstances, if the mean of the twotemperatures determined in glycerin 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.11.3 To convert softening poin
44、ts slightly above 80C176F determined in water to those determined in glycerin,the correction for asphalt is + 4.2C + 7.6F and for coal-tarpitch is + 1.7C + 3.0F. For referee purposes, repeat the testin a glycerin bath.11.3.1 Under any circumstances, if the mean of the twotemperatures determined in w
45、ater is 85.0C 185.0F orhigher, repeat the test in a glycerin bath.12. Report12.1 When usingASTM Thermometer 15C or 15F, report tothe nearest 0.2C or 0.5F the mean or corrected mean of thetemperatures recorded in 10.6 as the softening point.12.2 When using ASTM Thermometer 16C or 16F report tothe nea
46、rest 0.5C or 1.0F the mean or corrected mean of thetemperatures recorded in 10.6 as the softening point.12.3 Report the bath liquid used in the test.13. Precision and Bias13.1 With distilled water or USP glycerin, the followingcriteria shall be used for judging the acceptability of results(95 % prob
47、ability):13.1.1 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.313.1.2 Multilaboratory PrecisionThe multilabor
48、atorystandard 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.313.2 BiasThe procedure in Test Method D36 has no biasbecause the value of the softening point of the
49、 bitumen test isdefined in terms of this test method.14. Keywords14.1 asphalt; ball and ring; bitumen; coal tar; softeningpointASTM 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 rig
