1、Designation: D3461 97 (Reapproved 2012)D3461 14Standard Test Method forSoftening Point of Asphalt and Pitch (Mettler Cup-and-BallMethod)1This standard is issued under the fixed designation D3461; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、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.1. Scope Scope*1.1 This test method covers the determination of the softening point of asphalt and pitch
3、in the range from 5050 C to180C180 C by the cup-and-ball apparatus, and gives results comparable to those obtained by Test Method D36.NOTE 1If the softening point of asphalt by this Mettler cup-and-ball method fails to meet specified requirements, tests may be rerun using the TestMethod D36 (ring-an
4、d-ball) softening point apparatus as a referee method.NOTE 1If the softening point of asphalt by this Mettler cup-and-ball method fails to meet specified requirements, tests may be rerun using the TestMethod D36 (ring-and-ball) softening point apparatus as a referee method.1.2 This standard does not
5、 purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2
6、A314 Specification for Stainless Steel Billets and Bars for ForgingD36 Test Method for Softening Point of Bitumen (Ring-and-Ball Apparatus)D140 Practice for Sampling Bituminous MaterialsD4296 Practice for Sampling Pitch3. Summary of Test Method3.1 In this test method the softening point is defined a
7、s the temperature at which the specimen, suspended in a cylindrical cupwith a 6.5-mm 6.5 mm hole in the bottom and with a lead ball,8 mm 8 mm in diameter, centered on top of the sample in the cup, flows downward a distance of 19 mm to interrupt a light beam,as the sample is heated at a linear rate i
8、n air.4. Significance and Use4.1 Asphalt and pitch do not go through a solid-liquid phase change when heated, and therefore do not have true melting points.As the temperature is raised, they gradually soften or become less viscous. For this reason, the determination of the softening pointmust be mad
9、e by an arbitrary, but closely defined, method if the test values are to be reproducible.4.2 This test method is useful in determining the consistency as one element in establishing the uniformity of shipments orsources of supply.5. Apparatus5.1 A Mettler METTLER TOLEDO dropping point cell3 can be u
10、sed to determine softening points by this test method. Thesecommercially available instruments consist of a control unit with a digital temperature indicator, matched furnace, indicator with1 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuel
11、s, and Lubricantsand is the direct responsibility ofSubcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved Nov. 1, 2012Oct. 1, 2014. Published November 2012November 2014. Originally approved in 1976. Last previous edition approved in 20072012as D3461
12、97 (2007).(2012). DOI: 10.1520/D3461-97R12.10.1520/D3461-14.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3
13、 Available from the Mettler Toledo, Inc.,The sole source of supply of the apparatus known to the committee at this time is available from Mettler-Toledo, LLC., 1900Polaris Pkwy, Columbus, OH 43240, . If you are aware of alternative suppliers, please provide this information to ASTM International Hea
14、dquarters. Yourcomments will receive careful consideration at a meeting of the responsible technical committee,1 Balances and Instruments, 69 Princeton-Hightstown Rd., Hightstown, NJ08520-0071.which you may attend.This document is not an ASTM standard and is intended only to provide the user of an A
15、STM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as publishe
16、d by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1furnace built in or attached, sample cartridges, and accessories. The
17、 control unit automatically regulates the heating rate of thefurnace. The softening point is indicated on the readout, and the heating program stopped, when the sample flow triggers aphotocell detector. the softening point detection.Ageneral view of the components of the Mettler apparatus METTLER TO
18、LEDOsoftening point instrument is shown in Fig. 1. (old instrument) and Fig. 2 (new instrument).5.1.1 Integrated or Separate Control UnitThis The control unit shall provide a continuous, linear temperature increase from2525 C to 250C250 C at a rate of 2C/min. 2 C/min.Adigital readout shall indicate
19、the temperature to 0.1C 0.1 C throughout.5.1.2 Integrated or Separate Furnace UnitThis The furnace unit shall be capable of heating a specimen cup assembly,one ortwo sample cup assemblies, as described in 5.1.3, at a linear rate of 22 C 6 0.3C/min.0.3 Cmin. It shall include a sensingsystem capable o
20、f detecting the softening point with a precision of 0.1C.0.1 C.5.1.3 SpecimenSample Cup AssemblyAcup of chromium-plated brass, or of aluminum, or of stainless steel conforming to therequirements for Type 303 (UNS 530300) S30300) stainless steel as prescribed in Specification A314, with the dimension
21、s shownin Fig. 23. It shall be placed in the assembly so that the test specimen will flow pitch sample softening point will be detected whenit has flowed down a distance of 19 mm before interrupting a light beam and stopping the heating program as the softening pointis reached.mm.FIG. 1 General View
22、 of the Mettler FP-5/53METTLER TOLEDO FP90 Control Unit with Heater FP83HTD3461 1425.1.4 Lead BallA lead ball weighing 3.20 g 6 0.10 g. A32-caliber A 32-caliber lead shot is suitable for this purpose.FIG. 2 General View of the METTLER TOLEDO DP70FIG. 23 Specimen CupD3461 1436. Reagents6.1 Xylene, in
23、dustrial grade.7. Calibration of Mettler METTLER TOLEDO Apparatus7.1 This step, required only occasionally, is designed to establish that the temperature indicated by the instrument is inagreement with a known standard. A special cup with a bottom orifice of 2.8 mm is used instead of the one prescri
24、bed for thespecimen testing.testing of pitch.7.2 ReagentUse either analytical reagent or primary standard grade benzoic acid for thisthe calibration. As this material ishygroscopic,hygroscopic it must be stored in a tightly sealed container, and replaced with fresh material from a newly openedsupply
25、 if hydration or other contamination is suspected.D3461 1447.3 Procedure: ProcedureOld Instruments:7.3.1 Filling the SpecimenSample CupPlace the cup on a clean, flat surface. Add a small amount of benzoic acid crystals andpress down with a rod (4.5 (approximately 4.5 mm in diameter). Check that the
26、bottom orifice is completely filled. Refill and repeatthe pressing step until the cup is filled with benzoic acid. Remove any crystals from the exterior of the cup.7.3.2 HeatingPreheat the Mettler furnace to 121C, 121 C, and maintain it at that temperature. Place the cartridge assemblycontaining the
27、 benzoic acid in position in the furnace, taking care that the slits for the light beam are properly positioned. Waitfor temperature equilibration, that is, the furnace and the sample are in equilibrium at the preset temperature, but not less than the30 s after inserting the cartridge, start the aut
28、omatic heating cycle at 0.2C/min. 0.2 C/min. The temperature will rise steadily atthe correct rate until the drop point is reached, and then remain steady on the readout.7.3.3 CleaningImmediately remove the cartridge assembly. Check to determine that the specimensample has passed throughthe light be
29、am and no pretriggeringpre-triggering has occurred. If a malfunction is suspected, the entire procedure must berepeated. Inspect the apparatus carefully to ensure that no residue remains. Use a spatula shaped to the contour of the cup to removemost of the remaining acid from the cup and from the bot
30、tom of the cartridge. Wash the cup and cartridge in xylene, or othersuitable solvent, to remove the last traces of the residue.7.3.4 InterpretationIf the result is not 123.5 6 0.5C, repeat the test. If the second value is 0.6C above or below 123.5C,measure the dropping point of a fresh specimen of b
31、enzoic acid. If the deviation exceeds 0.6C, the instrument requiresrecalibration or repair. Consult the manufacturers instruction manual.7.4 InterpretationSee 7.6.7.5 ProcedureNew Instruments:7.5.1 Filling the Sample CupPlace the cup on a clean, flat surface. Optionally, the sample preparation tool
32、may be used. SeeFig. 2. Add a small amount of benzoic acid crystals and press down with a rod (approximately 4.5 mm in diameter). Check thatthe bottom orifice is completely filled. Refill and repeat the pressing step until the cup is filled with benzoic acid. Remove anycrystals from the exterior of
33、the cup. Place a glass collector below the cup and a cup cap on top, and place in the sample carrier.Two cup assemblies may be placed in the sample carrier.7.5.2 HeatingPreheat the furnace to 121 C and maintain it at that temperature. Place the sample carrier containing thebenzoic acid in position i
34、n the furnace. Wait for temperature equilibration, that is, the furnace and the sample are in equilibriumat the preset temperature, but not less than 30 s after inserting the cartridge, start the automatic heating cycle at 0.2 C/min. Thetemperature will rise steadily at the correct rate until the dr
35、op point is reached, and then remain steady on the readout. If there aretwo samples, heating will continue until both have dropped.7.5.3 CleaningImmediately remove the cartridge assembly. Check to determine that the sample has dropped and nopre-triggering has occurred. The video may be viewed to mak
36、e sure the drop was detected correctly. If a malfunction is suspected,the entire procedure must be repeated. Inspect the apparatus carefully to ensure that no residue remains. Use a spatula shaped tothe contour of the cup to remove most of the remaining acid from the cup. Wash the cup and glass coll
37、ector in xylene, or othersuitable solvent, to remove the last traces of the residue. Glass collectors may be treated as disposable items.Aluminum cups maybe used which may also be considered to be disposable.7.6 InterpretationIf the result is not 123.5 C 6 0.5 C, repeat the test. If the second value
38、 is 0.6 C above or below 123.5C, measure the dropping point of a fresh sample of benzoic acid. If the deviation exceeds 0.6 C, the instrument requiresrecalibration or repair. Consult the manufacturers instruction manual.8. Sampling8.1 Samples from shipments shall be taken in accordance with Practice
39、 D140 for asphalt and Practice D4296 for pitch and shallbe free of foreign substances. Thoroughly mix the sample before removing a representative portion for the determination or fordehydration.8.2 Pitch Sample Preparation:8.2.1 If a solid bulk sample contains free water, air-dry a representative po
40、rtion at 60C60 C or below.8.2.2 If the sample is liquid, check for any surface foam which may indicate the presence of water. If foam is found, maintainthe sample at a temperature of about 125C 125 C in an open container until the surface is free of foam. Take care not to overheat.Remove from the he
41、at source as soon as the foam has subsided. Proceed as directed in 9.1.8.2.3 Crush air-dry lumps of pitch to a size of 6 mm to 12 mm. 12 mm. Add the material to a container, having a height equalto or exceeding its width, and having a volume of not less than50 mL, 50 mL, until it is about half full.
42、 Place the container on a hot plate, or in an oven or a bath. Do not use an open flame formelting pitch. After melting is complete, stir gently but thoroughly, avoiding incorporation of air bubbles. The maximumtemperature of the molten pitch should not exceed the expected softening point by more tha
43、n 50C. 50 C. Any foam that formsmust be skimmed off.8.3 Asphalt Sample Preparation:D3461 1458.3.1 Heat the sample, with care to prevent local overheating, constantly stirring until it has become sufficiently fluid to pour.In no case, however, shall the temperature be raised more than 110C (200F) 110
44、 C (200 F) above the expected softening pointfor asphalt. Avoid incorporating air bubbles in the sample.8.3.2 Bring the asphalt sample to the pouring temperature in not more than 2 h.9. Test Specimen9.1 Prepare the test specimen by slightly overfilling the specimen cup, which rests on a brass plate.
45、 Optionally, the samplepreparation tool may be used (see Fig. 2). Keep the lip of the container close to the top of the cup to minimize entrainment of airbubbles. UnderpouringUnder-pouring past the blade of a spatula is helpful in this respect. Cool the specimen in the cup until firm,under cold wate
46、r if necessary. Trim the specimen flush with the top of the cup by pressing with a heated knife or spatula whiledrawing it toward you. Support the cup with tweezers or forceps or in a wood block with holes sized to fit the cup. Do not trimby cutting across the top with a forward or sideward motion a
47、s this tends to lift the specimen out of the mold, thus creating aninternal void which is not easily detected, and which significantly alters the result.9.2 An alternative method which avoids possible loss of volatiles in remelting,re-melting, is to press the cold, solid specimeninto the specimen cu
48、p. Select clean, dry, dust-free lumps from the representative portion of the sample and crush to a size of lessthan 2 mm. Place a sample cup in the mold (see Fig. 34, Fig. 45, and Fig. 56). Place the assembled mold, with the knockout pinin position, on the bottom plate of a hydraulic press. Pour abo
49、ut 2 g of the crushed specimen into the top of the mold and insertthe top ram. Compress the specimen into the cup with a total force on the ram of 22.24 kN (5000 lbf).lb). Hold this pressure fora minimum of 15 s. Excessive molding pressure can cause the specimen cup to fail by shearing. Remove the mold assembly fromthe press and rotate the upper half while keeping the lower half of the mold stationary. This action causes the specimen to shearhorizontally at the top of the cup. Separate the two parts of th
