1、Designation: D2319/D2319M 98 (Reapproved 2013)Standard Test Method forSoftening Point of Pitch (Cube-in-Air Method)1This standard is issued under the fixed designation D2319/D2319M; the number immediately following the designation indicates theyear of original adoption or, in the case of revision, t
2、he year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the soft-ening point above 80C 176F of pitch. Test Method D310
3、4gives comparable results.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 exact equivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems may resu
4、lt 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 user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory l
5、imitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D61 Test Method for Softening Point of Pitches (Cube-in-Water Method)D3104 Test Method for Softening Point of Pitches (MettlerSoftening Point Method)D4296 Practice for Sampling PitchE1 Specification for ASTM Liquid-in-Glass Thermomet
6、ers3. Summary of Test Method3.1 Two cubes of pitch, supported on wire hooks, are heatedin a standardized air oven at a linear rate. The softening pointis the mean of the temperatures at which the cubes sagdownwards a distance of 60 mm 2.4 in.4. Significance and Use4.1 Pitch does not go through a sol
7、id-liquid phase changewhen heated and therefore does not have a true melting point.As the temperature is raised, pitch softens and becomes lessviscous. The softening point is arbitrarily defined and must bedetermined by a closely controlled method that must becarefully followed if test results are t
8、o be reproducible.4.2 This test method is useful in determining the consis-tency of pitch as one element in establishing the uniformity ofshipments and sources of supply.5. Apparatus35.1 Air OvenThe oven shall be cylindrical, 150 mm 6 in.in inside diameter by 155 mm 6.2 in. in height. It shall havet
9、wo 75 mm 3-in. diameter windows of mica, centeredvertically on opposite sides, and shall be fitted with a coverhaving a central opening 25 mm 1 in. in diameter to hold athermometer, and a concentric ring suspended below to supportthe hooks with attached specimens. The ring shall be made of6mm14-in.
10、brass, shall be 54 mm 218 in. in outsidediameter, and shall be centrally suspended 30 mm 1.2 in.below the cover. The cover shall have two 3 mm 0.12-in.holes on a diagonal 50 mm 2 in. from the center. On thebottom of the oven, an inner pan 140 mm 5.6 in. in diametershall rest on three brass legs 5 mm
11、 0.2 in. in height fastenedto the bottom of the pan to provide an air space between thepan and the bottom of the oven. The side wall, cover, and panshall be made of 0.7 mm 0.028 in. thick or 22-gauge (BWG)copper sheet, and the bottom of 0.8 mm 0.032 in. thick or21-gauge copper.5.2 Tripod for Use wit
12、h Gas BurnerThe tripod ring shallbe approximately 125 mm 5 in. in inside diameter so that theoven is supported only on its outer edges. It shall be 200 mm8 in. in height.5.3 Shield for Oven:5.3.1 For Use with Electric HeaterThe shield shall becylindrical, 216 mm or 8.64 in. in inside diameter by 181
13、 mmor 714 in. in height. It shall have two 76 mm or 3-in.diameter mica windows on opposite sides, positioned to1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels, Petroleu
14、m Coke and Carbon Material.Current edition approved July 15, 2013. Published August 2013. Originallyapproved in 1964. Last previous edition approved in 2008 as D2319 98 (2008)1.DOI: 10.1520/D2319_D2319M-98R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Custom
15、er Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The sole source of supply of the softening point apparatus items, obtainable asa unit on special order, known to the committee at this time is Humboldt
16、Manufacturing Co., 7302 W. Agatite Ave., Chicago, IL 60656. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend. All othe
17、r apparatus itemsdescribed may be obtained from any regular laboratory equipment supply house.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1coincide with the windows of the oven when both are placed onthe electric heater. It shall b
18、e made of 0.7 mm 0.028 in. thickor 22-gauge sheet metal, painted inside and out with aluminumpaint.5.3.2 For Use with Gas BurnerThe shield shall be iden-tical with that described in 5.3.1 except that it shall be 375 mm15 in. in height and the windows shall coincide when theshield is standing on the
19、bench and the oven on the tripoddescribed in 5.2. A door 115 by 115 mm 412 by 412 in. shallbe provided at the bottom to give access to the burner.5.4 MoldA mold suitable for forming two 12.7 mm12-in. cubes of pitch, having cylindrical core pins 12 gauge2.05 to 2.07 mm in diameter located in the base
20、 plate of theassembly to produce accurately centered suspension holes inthe cubes. See Fig. 1 of Test Method D61 for details.5.5 HooksTwo L-shaped hooks made of 2.06 mm or12-gauge copper wire. The foot of the hook shall be 25 mm 1in. in length and at a right angle to the upright portion forinsertion
21、 into the central hole of the pitch cube. The uprightportion shall have a partial loop at the top to fit over the supportring, and shall be of the proper length, approximately 50 mm2 in., to position the foot on an imaginary line runninghorizontally through the center of the windows.5.6 ThermometerA
22、STM High-Softening PointThermometer, having a range from 30 to 200C 80 to 400F,and conforming to the requirements for Thermometer 16C asdescribed in Specification E1.5.7 Heat Source:5.7.1 Electric HeaterA hot plate provided with a variabletransformer or other device for regulating the temperature of
23、the heating element. It should be shielded from drafts on threesides.5.7.2 Gas Burner, bunsen-type, with a chimney and asensitive valve for regulating the size of the flame.6. Bulk Sampling6.1 Samples from shipments shall be taken in accordancewith Practice D4296 and shall be free of foreign substan
24、ces.Thoroughly mix the sample before removing a representativeportion for the determination or for dehydration.7. Dehydration7.1 If the bulk sample contains free water, air-dry a repre-sentative portion in a forced draft oven at 50C.8. Test Specimens8.1 To melt a solid pitch sample, add the material
25、 to acontainer having a height equal to or exceeding its width, anda volume of not less than 50 mL, until it is about half full. Placethe container on a hot plate, or in an oven or bath. Do not usean open flame for melting pitch. After melting is complete, stirthoroughly but gently with the thermome
26、ter or glass rod,avoiding the incorporation of air bubbles. The maximumtemperature shall not exceed the expected softening point bymore than 50C 90F. Any foam that may form must beskimmed off the surface.8.2 Coat the inner surfaces and core pins of the mold lightlywith silicone oil or silicone greas
27、e. Pour molten pitch into thecavities of the mold with the lip of the container close to thesurface to minimize entrainment of air bubbles. Underpouringpast the blade of a spatula is helpful in this respect. Even smallbubbles markedly effect the weight of the cube and theobserved softening point. Us
28、e an excess of pitch to allow forshrinkage on cooling. Cool in the mold until firm, and removethe surplus by drawing the heated blade of a putty-knife orspatula across the surface of the mold so that the cubes arepressed into the cavities. Open the mold and remove the cubescarefully. Inspect each sp
29、ecimen for possible cracks or bubblesand reject any which are imperfect. To reduce the risk ofcracking, the mold may be heated to a temperature 50C 90Fbelow the expected softening point before the specimens arepoured.8.3 Place two cubes of pitch on hooks, as shown in Fig. 1 ofTest Method D61, warmin
30、g the hooks slightly if necessary. Thefoot of the hook passes through the center of two oppositefaces, while the other four shall be at an angle of 45 to thehorizontal. The shaft of the hook shall be 3 to 5 mm 0.1 to 0.2in. from the specimen.9. Preparation of Apparatus9.1 Assemble the apparatus in a
31、n area free of drafts.9.2 Ensure that the oven, cover, and pan are clean, bright,and free of dents, since tarnished or dirty apparatus maychange the apparent softening point. After each determination,carefully clean the hooks with a solvent for pitch. Avoidscraping or other mechanical methods that m
32、ay alter thediameter of the wire, which shall be checked frequently forconformance with the specified 2.05 to 2.07 mm 0.082 in.diameter.9.3 Set the pan on its legs on the bottom of the oven. Centerit so that the space for air circulation is approximately equal allaround the circumference. Place a si
33、ngle 110 mm 4.4 in. filterpaper on the pan.9.4 Specimens and oven are normally at room temperature.For harder pitches, the oven may be preheated to a temperaturenot higher than 60C 108F below the expected softeningpoint.10. Procedure10.1 Suspend the hooks with the test specimens in placefrom the sup
34、porting ring on the oven cover with the tips of thehooks pointing toward each other from the left and right sidesof the thermometer as viewed through the windows. The feet ofthe hooks shall lie along an imaginary horizontal line throughthe center of the windows.10.2 Insert the thermometer through a
35、cork in the centralhole in the cover so that the bottom of the bulb is level with thebottom edges of the cubes, and the ends of the feet of the hooksare close to, but do not touch, the bulb.10.3 Center the oven on the heat source and place the shieldaround it so that the two are concentric.D2319/D23
36、19M 98 (2013)210.4 Preheat the oven if necessary and, when equilibrium isestablished, adjust the heating rate so that the temperature risesat 5C/min 10F/min. The maximum permissible variationfrom this rate shall be 61.0C/min 62F/min for the final50C 90F below the softening point.10.5 Maintain a writ
37、ten record of the temperature to 0.25C0.5F for each minute over the last 50C 90F. Averagethese readings algebraically. The average shall not deviatemore than 60.5C 61F from the 5C/min 10F/min overthis interval. Reject any test in which the rate for any minute inthis interval is outside the range fro
38、m 4 to 6C 7 to 11F, orthe average is outside the range from 4.5 to 5.5C 8 to 10F.10.6 The softening point is the average of the thermometerreadings (with no correction for emergent stem) when the twocubes touch the pan. Estimate the readings to 0.25C 0.5F.If the individual values differ by more than
39、 1.5C 2.7F,reject the result and repeat the test.11. Report11.1 Report the average as the softening point to the nearest1F. If the result is required in degrees Celsius, report to thenearest 0.5C.12. Precision and Bias12.1 The following criteria shall be used to judge theacceptability of results (95
40、 % confidence level) for softeningpoint (cube-in-air):12.1.1 RepeatabilityDuplicate results by the same opera-tor shall not be considered suspect unless they differ by morethan 1.0C 2F.12.1.2 ReproducibilityThe values reported by each of twolaboratories, representing the arithmetic average of duplic
41、atedeterminations, shall not be considered suspect unless theydiffer by more than 7.2F 4.0C.12.1.3 BiasThis procedure has no bias because the valueof softening point is defined in terms of this test method.13. Keywords13.1 cube-in-air; pitch; softening pointASTM International takes no position respe
42、cting 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 such rights, are entirely their own responsibility.This st
43、andard 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 additional standardsand should be addressed to ASTM Internat
44、ional 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 the ASTM Committee on Standards, at the address shown belo
45、w.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/).D2319/D2319M 98 (2013)3
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