ASTM D36 D36M-2014e1 Standard Test Method for Softening Point of Bitumen &40 Ring-and-Ball Apparatus&41 《沥青软化点的标准试验方法(环球仪法)》.pdf

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1、Designation: D36/D36M 141Standard 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 re

2、vision. A number in parentheses indicates the year of last reapproval.A superscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTETable 1 was editorially corrected in August 2014.1. Scope1.1 This test method covers the determination of the soft-ening point of bi

3、tumen 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 ineach system may not be exa

4、ct 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 is theresponsibility of the

5、 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 Construction MaterialsD92 Test

6、 Method for Flash and Fire Points by ClevelandOpen Cup TesterD140 Practice for Sampling Bituminous MaterialsD3461 Test Method for Softening Point of Asphalt and Pitch(Mettler Cup-and-Ball Method)E1 Specification for ASTM Liquid-in-Glass ThermometersE177 Practice for Use of the Terms Precision and Bi

7、as inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. 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 sof

8、tening point is reported as themean of the temperatures at which 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 a

9、nd lessviscous as the temperature rises. For this reason, softeningpoints 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 so

10、urces of supply, and is indicative of thetendency of the material 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 PlateA flat, smooth, brass plate approxi-mately 50 by 75 mm 2 by

11、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 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, n

12、ot 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 heat-resistant glassmeets this requirement.5.6 Ring Holder and AssemblyA brass holder designed tosupport the two rings in a horizontal position, conforming t

13、othe shape and dimensions shown in Fig. 1 (c), supported in theassembly illustrated in Fig. 1 (d). The bottom of the shoulderedrings in the ring holder shall be 25 mm 1.0 in. above the1This test method is under the jurisdiction of ASTM Committee D08 on Roofingand Waterproofing and is the direct resp

14、onsibility of Subcommittee D08.03 onSurfacing and Bituminous Materials for Membrane Waterproofing and Built-upRoofing.Current edition approved July 1, 2014. Published July 2014. Originally approvedin 1962. Last previous edition approved in 2012 as D36 12. DOI: 10.1520/D0036_D0036M-14E01.2For referen

15、ced 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Co

16、nshohocken, PA 19428-2959. United States1upper 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 to t

17、herequirements 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 thethermometer specified in Specification E1,(2) capable ofindicating temperature to within 1C 2F, and (3) stable towit

18、hin 1C 2F for the duration of the exposure.5.7.2 An ASTM High Softening 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 leas

19、t: (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.5.7.3 The appropriate thermometer shall be suspended inthe assembly as shown in Fig. 1 (d) so that the

20、 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.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 t

21、he thermometer specifiedin Specification E1,(2) capable of 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 e

22、ssential to avoidtrapping air bubbles on the surface of the specimen which may affect theresults.6.1.2 USP Glycerin. (WarningGlycerin has a flash pointof 160C 320F in accordance with Test Method D92.)NOTE 1All dimensions are in millimetres (60.3 mm except where noted).FIG. 1 Shouldered Ring, Ball-Ce

23、ntering Guide, Ring Holder, and Assembly of Apparatus Showing Two RingsD36/D36M 14126.2 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 glyc

24、erin 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 can produceerroneous results in other tests s

25、uch as those for penetrationand flash point.)7. Hazards7.1 WarningMercury has been designated by EPA andmany state agencies as a hazardous material that can causecentral nervous system, kidney, and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution shou

26、ld be taken when handling mercury andmercury containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAs website,http:/www.epa.gov/mercury/faq.htm, for additional informa-tion. Users should be aware that selling mercury or mercurycontaining products, or bo

27、th, 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 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 b

28、itumen 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-surface-area ratio of 37 kW/m2has been found

29、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 above 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

30、 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 thissample; 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

31、 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 eachring, 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

32、 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.9.4 When the specimens have cooled, cut away the excessbitumen cleanly with a slightly heated knife or

33、 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 appropriate for the expected softening point:10.1.1 Freshly boiled distilled water for softening pointsbetween 30 and 80C 86 and 176F; use Thermometer 1

34、5C 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 Thermometer 16C or16F or the thermometric device. The starting bath temperatureshall be no higher than 30 6 1C 86 6 2F.10.1.3 For referee purposes, all softe

35、ning 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 apparatus in the laboratory hood with thespecimen rings, ball-centering guides, and thermometer inposition,

36、 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 for at least5 min so they will reach the same starting temperature as therest of the assembly.10.3 Place the bath in ice water, if ne

37、cessary, 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 the bottom ofthe bath in each ball-centering guide.10.5 Heat the bath from below so tha

38、t 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. The maximum permissible variation for any1-min period after the first 3 min shall be 6

39、0.5C 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 burner or electric heater may beused, but the latter must be of the low-lag, variable output

40、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 correction for theemergent stem of the thermometer. If the difference betweenthe two temperat

41、ures 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 determination isnecessarily arbitrary, this difference matters only for softeningpoints

42、slightly above 80C 176F.11.2 The change from water to glycerin for softening pointsabove 80C creates a discontinuity. With rounding, the lowestD36/D36M 1413possible asphalt softening point reported in glycerin is 84.5C184F, and the lowest possible coal-tar pitch softening pointreported in glycerin i

43、s 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, and forcoal-tar pitch is 1.7C 3.0F. For referee purposes, repeatthe test in a water bath.11.2.2 Under any cir

44、cumstances, 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 points slightly above 80C176F determined in water to those determined in glycerin,the corre

45、ction 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 water is 85.0C 185.0F orhigher, repeat the test in a glycerin bath.12. Report12.1 When using

46、ASTM 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 nearest 0.5C or 1.0F the mean or corrected mean of thetemperatures recorded in 10.6 as the sof

47、tening point.12.3 Report the bath liquid used in the test.13. Precision and Bias313.1 The precision of this test method is based on aninterlaboratory study of Test Method D36/D36M, StandardTest Method for Softening Point of Bitumen (Ring-and-BallApparatus), conducted in 2012. In this study, ten labo

48、ratorieswere asked to test three different materials. Every “test result”represents the average of two individual determinations, and allparticipants were instructed to report triplicate test results.Practice E691 was followed for the design and analysis of thedata; the details are given in ASTM Res

49、earch Report No.D08-1017.313.1.1 Repeatability (r)The difference between repetitiveresults obtained by the same operator in a given laboratoryapplying the same test method with the same apparatus underconstant operating conditions on identical test material withinshort intervals of time would in the long run, in the normal andcorrect operation of the test method, exceed the followingvalues