1、Designation: D6493 05 (Reapproved 2010)Standard Test Methods forSoftening Point of Hydrocarbon Resins by Automated Ring-and-Ball Apparatus1This standard is issued under the fixed designation D6493; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e 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*1.1 These test methods are intended for determining thesoftening point of hydrocarbon resins a
3、nd similar materials bymeans of an automated ring-and-ball apparatus. Portions aresimilar in technical content to the automated-apparatus ver-sions of Test Methods D36, E28, and ISO 4625.1.1.1 The ring-and-ball softening point of a hydrocarbonresin may also be determined with lower precision using t
4、hemanual ring-and-ball softening point procedure in Test Meth-ods E28.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard method does not purport to address all ofthe safety concerns, if any, associated with i
5、ts 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:2D36 Test Method for Softening Point of Bitumen (Ring-and-Ball Apparatu
6、s)E1 Specification for ASTM Liquid-in-Glass ThermometersE28 Test Methods for Softening Point of Resins Derivedfrom Naval Stores by Ring-and-Ball ApparatusE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Pre
7、cision of a Test Method2.2 ISO Standard:ISO 4625 Binders for paints and varnishesDeterminationof softening pointRing-and-ball method33. Summary of Test Method3.1 These test methods are for the determination of ahydrocarbon resins softening pointthe temperature at whicha disk of the resin held within
8、 a horizontal ring is forceddownward a distance of 25.4 mm (1.00 in.) under the weight ofa standard steel ball, as the specimen is heated at 5C/min. ina specified liquid bath.4. Significance and Use4.1 For hydrocarbon resins, softening does not take place ata definite temperature.As the temperature
9、rises, these materialsgradually change from brittle solids or very viscous liquids toless viscous liquids. For this reason, determination of thesoftening point must be made by a fixed, arbitrary, and closelydefined method if the results obtained are to be comparable.5. Sample Preparation5.1 Preparat
10、ion of Sample by the Pour Method: Thisprocedure is suitable for resins that can be heated and pouredwithout adverse effect on the softening point.5.1.1 Select a sample representative of the material to betested. The sample should consist of flakes, pastilles, or brokenlumps. Avoid inclusion of finel
11、y divided material or dust.5.1.2 Select a quantity of resin having a volume at leasttwice that necessary to fill the desired number of rings, andmelt it in a clean container, using an oven, hot plate, sand bathor oil bath to prevent local overheating. If necessary, stirslowly, taking care to avoid i
12、ncorporating air bubbles in thesample. Melt the sample completely, but do not heat it above atemperature necessary to pour the material readily. The timefrom the beginning of heating to pouring should not exceed 15min.5.1.3 For materials that tend to crack or shrink in the ring oncooling, immediatel
13、y before filling the ring, preheat the ring toapproximately the temperature at which the material is to bepoured. The ring, while being filled, should rest bottom down1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and ar
14、e the directresponsibility of Subcommittee D01.34 on Pine Chemicals and HydrocarbonResins.Current edition approved July 15, 2010. Published September 2010. Originallyapproved in 1999. Last previous edition approved in 2005 as D6493 05. DOI:10.1520/D6493-05R10.2For referenced ASTM standards, visit th
15、e 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.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY
16、10036, http:/www.ansi.org.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.(see Fig. 1(a) on a suitable metal surface. Pour the sample intothe ring so as to leave an ex
17、cess on cooling. After cooling aminimum of 30 min., trim off the excess resin from the top andoutside of the ring. To remove excess resin from the top, cut theexcess off cleanly with a heated knife or spatula, or grasp thering in a pair of tongs and draw the top surface quickly andfirmly over the su
18、rface of a heated plate.NOTE 1If the determination is repeated, us a clean container and afresh sample.5.2 Preparation of Sample by the Powder Method: Thisprocedure is suitable for high softening-point materials thatcannot be heated and poured without adverse effects on thesoftening point. See Appen
19、dix X1.1, Alternate Sample Prepa-ration Procedures.5.3 Preparation of Samples Having a Low Softening Point(up to 35C (95F):5.3.1 Place a ring on a piece of aluminum foil. Pour thematerial to be tested into the ring, then place the foil and thefilled ring on dry ice or in a freezer to cool. The mater
20、ial in thering must be free of bubbles.5.3.2 After cooling, cut and scrape off any excess materialusing a slightly heated spatula, then slide the ring gently fromthe foil. Place the ring in the supporting apparatus, and performthe softening point determination in accordance with Section12.6. Apparat
21、us6.1 Automated Ring-and-Ball Softening Point Instrument,having a test assembly consisting of: a ring holder, a metalplate, and a cover mounted on two support rods (see Fig. 1(b)and (d), a temperature-measuring device (in accordance withSpecification E1), a heating unit, a heating-rate controller, a
22、nda digital temperature display.6.2 RingA brass, shouldered ring conforming to thedimensions shown in Fig. 1(a).6.3 BallA steel ball, 9.53 6 0.1 mm (38 in.) in diameter,weighing between 3.45 and 3.55 g.6.4 Ball-Centering Guide (optional), having the dimensionsgiven in Fig. 1(c).FIG. 1 Shouldered Rin
23、g, Ring Holder, Ball-Centering Guide, and Assembly of ApparatusD6493 05 (2010)26.5 Beaker, 600 mL, borosilicate glass, to hold the bathliquid. ensure that the dimensions will properly fit the heatingunit.6.6 StirrerEither a magnetic stirring motor and a mag-netic stir bar, or a direct-driven agitato
24、r with a stirring motor.The dimensions of a stir bar must be such that the bar spinsfreely under the test assembly. The bath must be stirred at aspeed sufficient to ensure uniform temperature distributionwithout causing significant sideways displacement of the resinas it sags below the ring.7. Reage
25、nts and Materials7.1 Bath Liquids:7.1.1 Distilled or Deionized Water, Freshly BoiledForsoftening points between 35C (95F) and 80C (176F).7.1.1.1 Use distilled or deionized water that has been cooledto at least 27C (81F) below the anticipated softening point,but in no case lower than 5C (41F).7.1.2 U
26、SP GlycerinFor softening points between 80C(176F) and 150C (302F). Repeated use of glycerin (overabout four heating cycles) may affect results. Open storage ofglycerin can increase the moisture content, which may affectresults. Replace with fresh glycerin if any change in appear-ance or viscosity is
27、 noted. Use fresh glycerin for referee work.WarningGlycerin must not be used for softening pointsgreater than 150C (302F) due to the 160C (320F) flashpoint of glycerin.7.1.3 Silicone Oil (Polydimethylsiloxane)For softeningpoints above 80C (176F). The oil must have a temperaturerange of 60 to 200C+ (
28、140 to 392F+), remain clear through-out the temperature range, have no apparent effect or reactivitywith the test specimen, remain free of moisture, and maintaina relatively uniform viscosity and stirring rate within thetemperature range.4NOTE 2Replace with fresh silicone oil if any change in appear
29、ance isnoted. Do not use silicone oil that contains any gels; gels are an indicatorthat degradation has occurred.7.1.4 Ethylene GlycolFor softening points up to 35C(95F).7.1.4.1 Prepare a fresh 50/50 (volume/volume) mixture ofdistilled water and ethylene glycol prior to softening pointdetermination.
30、 Alternatively, for softening points between 0Cand 35C, a 50/50 (v/v) mixture of glycerin and water may beused.8. Calibration8.1 The calibration of any automated ring and ball softeningpoint apparatus must be performed on a regular basis, sinceaccurate temperature control is required. Follow the man
31、ufac-turers instructions for calibration of the instrument.9. Procedure for Materials Having a Softening PointBetween 35C (95F) and 80C (176F)9.1 Add a stir bar or stirrer to the 600-mL beaker. Addapproximately 500 mL of water, conforming to the require-ments in 7.1.1. Ensure that the beaker is prop
32、erly positioned onthe heater in the test unit. Place the prepared sample rings inthe test assembly. Place a ball-centering guide and ball on topof each sample ring. Place the test assembly in the beaker.Place the temperature-measuring device in the opening in thecover of the test assembly. Verify th
33、at the control unit is set forthe correct bath liquid.9.2 Heat the bath so that the temperature of the water israised uniformly at a rate of 5C (10F)/min. Protect the bathfrom drafts, using shields if necessary. Reject any test in whichthe rate of temperature rise does not fall within these limits.T
34、he test is complete when the light beam has been interruptedby the falling ball and material.NOTE 3Rigid adherence to the prescribed rate of heating is absolutelyessential for reproducibility of results.9.3 Record as the softening point the temperature displayedon the unit after the light beam has b
35、een interrupted by thefalling ball and material.9.4 Start the cooling process in the instrument. Remove thetemperature measuring device from the test insert, then removethe test insert from the beakers. Thoroughly clean the testinsert, ball, and ring in a suitable solvent.10. Procedure for Materials
36、 Having Softening PointsBetween 80C (176F) and 150C (302F)10.1 Use the same procedure as described in Section 9,except fill the bath with glycerin or silicone oil.NOTE 4For materials softening around 80C (176F) report the bathliquid used, since a glycerin or silicone oil bath will yield a slightly h
37、igherresult than a water bath.11. Procedure for Materials Having Softening PointsAbove 150C (302F)11.1 Use the same procedure as described in Section 9,except fill the bath with silicone oil (see Note 2).12. Procedure for Materials Having Softening PointsBelow 35C (95F)12.1 Additional Apparatus:12.1
38、.1 Isopropyl Alcohol Dry Ice Bath.12.2 Procedure:12.2.1 Cool the beaker containing the liquid bath, describedin 7.1.4.1, to 25C (13F) in an isopropyl alcohol/dry icebath.12.2.2 Use the same procedure as in Section 9 except for thebath liquid, and begin heating as directed once the testspecimen in th
39、e ring has been placed in the bath.13. Report13.1 Report the softening point to the nearest 1C.13.2 Report the bath liquid used in the test.14. Precision and Bias414.1 An interlaboratory study of the ring-and-ball softeningpoint of three hydrocarbon resins was run in 1998 by 23laboratories. The desi
40、gn of the study, similar to that of PracticeE691, and an analysis of the data are given in ASTM ResearchReport No. RR:D01-1113. The precision values given for4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1113.D6493 05 (201
41、0)3ring-and-ball softening point of hydrocarbon resins are for thecomparison of two test results (single determinations).14.1.1 For a material having a 70C ring-and-ball softeningpoint, run in a water bath:14.1.1.1 Repeatability Limit 95 % (within laboratory): Thedifference between two results obtai
42、ned by the same operatorwith the same apparatus on identical test material shall, at the95 % confidence level, not exceed 0.7C.14.1.1.2 Reproducibility Limit 95 % (between laboratories):The difference between two results obtained by differentoperators with different apparatus on identical test mater
43、ialshall, at 95 % confidence level, not exceed 3.9C.14.1.2 For a material having a 100 to 135C ring-and-ballsoftening point, run in a glycerin or silicon oil bath:Repeatability Limit 95 % (within laboratory) = 1.8C.Reproducibility Limit 95 % (between laboratories) = 4.6C.14.2 These terms (repeatabil
44、ity limit and reproducibilitylimit) are used as specified in Practice E177. The respectivestandard deviations among test results, related to the abovenumbers by the factor 2.8, are as follows:14.2.1 For a material having a 70C ring-and-ball softeningpoint, run in a water bath:Repeatability Standard
45、Deviation = 0.3C.Reproducibility Standard Deviation = 1.4C.14.2.2 For a material having a 100 to 135C ring-and-ballsoftening point, run in a glycerin or silicone oil bath:Repeatability Standard Deviation = 0.7C.Reproducibility Standard Deviation = 1.7C.14.3 BiasSince there is no accepted reference m
46、aterial,method or laboratory for determining the bias for the procedurein these test methods for measuring the ring-and-ball softeningpoint, no statement on bias can be made.15. Keywords15.1 hydrocarbon resin; ring and ball; softening pointAPPENDIX(Nonmandatory Information)X1. ALTERNATIVE SAMPLE PRE
47、PARATION PROCEDUREX1.1 Preparation of Sample by the Powder Method:X1.1.1 This sample preparation procedure is suitable formaterials that cannot be melted and poured without altering thesoftening point.X1.1.2 ApparatusFor the powder method of samplepreparation the following additional apparatus is re
48、quired:X1.1.2.1 RingAs an alternative to the brass ring conform-ing to the dimensions shown in Fig. 1(a); a ring made of steelmay be used to minimize the possibility of its deformationduring the compacting operation.X1.1.2.2 Ring Support and PestleAsteel pestle and a ringsupport consisting of: sleev
49、e, knock-out-button, ring support,and cup-shaped “mortar,” conforming to the dimensions shownin Fig. X1.1.X1.1.2.3 PressA hydraulic press or any other suitablepress capable of maintaining sustained pressures up to 55 MPa(8000 psi).X1.1.3 Procedure:X1.1.3.1 Select a sample as described in 5.1.1 and break upthe pieces until there are no particles larger than 3 mm (18 in.).Mix the material thoroughly, and quarter down until a suitablequantity (approximately 50 to 75 g) is obtained for powdering.X1
