1、Designation: D6493 11Standard Test Methods forSoftening Point of Hydrocarbon Resins and Rosin BasedResins 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
2、 case 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 resi
3、ns, rosin based resins andsimilar materials by means of an automated ring-and-ballapparatus. Portions are similar in technical content to theautomated-apparatus versions of Test Methods D36, E28, andISO 4625.1.1.1 The ring-and-ball softening point of a hydrocarbonresin and rosin based resins may als
4、o be determined with lowerprecision using the manual ring-and-ball softening point pro-cedure in Test Methods 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 ofth
5、e safety 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 limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D36 Test Method for Soften
6、ing Point of Bitumen (Ring-and-Ball Apparatus)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
7、an Interlaboratory Study toDetermine the Precision 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 thesoftening pointthe temperature at which a d
8、isk of the resinheld within a horizontal ring is forced downward a distance of25.4 mm (1.00 in.) under the weight of a standard steel ball, asthe specimen is heated at 5C/min. in a specified liquid bath.4. Significance and Use4.1 For hydrocarbon resins and rosin based resins, softeningdoes not take
9、place at a definite temperature. As the tempera-ture rises, these materials gradually change from brittle solidsor very viscous liquids to less viscous liquids. For this reason,determination of the softening point must be made by a fixed,arbitrary, and closely defined method if the results obtained
10、areto be comparable.5. Sample Preparation5.1 Preparation 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
11、, pastilles, or brokenlumps. Avoid inclusion of finely 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 overheat
12、ing. If necessary, stirslowly, taking care to avoid incorporating 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
13、 to crack or shrink in the ring oncooling, immediately 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 down(see Fig. 1(a) on a suitable metal surface. Pour the sample intothe ring so as t
14、o leave an excess on cooling. After cooling a1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.34 on Pine Chemicals and HydrocarbonResins.Current edition approved June 1,
15、 2011. Published June 2011. Originallyapproved in 1999. Last previous edition approved in 2010 as D6493 05 (2010).DOI: 10.1520/D6493-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume in
16、formation, 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 10036, http:/www.ansi.org.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 1
17、00 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.minimum 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
18、 draw the top surface quickly andfirmly over the surface 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 witho
19、ut adverse effects on thesoftening point. See Appendix 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
20、 ring on dry ice or in a freezer to cool. The material 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 de
21、termination in accordance with Section12.6. Apparatus6.1 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 built in digital temperature that should be standard-ized pe
22、riodically to ensure that it meets the specifications forand gives the same readings as thermometers given in Speci-fication E1, a digital temperature display, a heating unit and aheating-rate controller.6.2 RingA brass, shouldered ring conforming to thedimensions shown in Fig. 1(a).6.3 BallA steel
23、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 Ring, Ring Holder, Ball-Centering Guide, and Assembly of ApparatusD6493 1126.5 Beaker, 600 mL, borosilicate glass, to hold the bath
24、liquid. 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 agitator 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 st
25、irred at aspeed sufficient to ensure uniform temperature distributionwithout causing significant sideways displacement of the resinas it sags below the ring.7. Reagents and Materials7.1 Bath Liquids:7.1.1 Distilled or Deionized Water, Freshly BoiledForsoftening points between 35C (95F) and 80C (176F
26、).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 USP GlycerinFor softening points between 80C(176F) and 150C (302F). Repeated use of glycerin (overabout four heating cycles) may affect
27、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 noted. Use fresh glycerin for referee work.WarningGlycerin must not be used for softening pointsgreater than 150C (302F) due to the 16
28、0C (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+ (140 to 392F+), remain clear through-out the temperature range, have no apparent effect or reactivitywith the test specimen, remain free
29、 of moisture, and maintaina relatively uniform viscosity and stirring rate within thetemperature range.4NOTE 2Replace with fresh silicone oil if any change in appearance isnoted. Do not use silicone oil that contains any gels; gels are an indicatorthat degradation has occurred.7.1.4 Ethylene GlycolF
30、or 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. Alternatively, for softening points between 0Cand 35C, a 50/50 (v/v) mixture of glycerin and water may beused.8. Calibration8.1 The ca
31、libration of any automated ring and ball softeningpoint apparatus must be performed on a regular basis, sinceaccurate temperature control is required. Follow the manufac-turers instructions for calibration of the instrument.9. Procedure for Materials Having a Softening PointBetween 35C (95F) and 80C
32、 (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 properly positioned onthe heater in the test unit. Place the prepared sample rings inthe test assembly. Place a ball-centering guide and ba
33、ll 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 that 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 ra
34、te 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.The test is complete when the light beam has been interruptedby the falling ball and material.NOTE 3Rigid adherence to the prescribed ra
35、te 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 been interrupted by thefalling ball and material.9.4 Start the cooling process in the instrument. Remove thetemperature measuring device
36、 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 Having Softening PointsBetween 80C (176F) and 150C (302F)10.1 Use the same procedure as described in Section 9,except fill the bath wi
37、th 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 higherresult than a water bath.11. Procedure for Materials Having Softening PointsAbove 150C (302F)11.1 Use the same procedure as descri
38、bed 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:12.1.1 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) i
39、n 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 the 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
40、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 design of the study, similar to that of PracticeE691, and an analysis of the data are given in ASTM ResearchReport No. RR:D01-1113. The pre
41、cision values given for4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1113.D6493 113ring-and-ball softening point of hydrocarbon resins are for thecomparison of two test results (single determinations). Similarprecision can
42、 be expected with rosin based resins.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 obtained by the same operatorwith the same apparatus on identical test material shall, at
43、 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 materialshall, at 95 % confidence level, not exceed 3.9C.14.1.2 For a material having a 1
44、00 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 (repeatability limit and reproducibilitylimit) are used as specified in Practice E177. The resp
45、ectivestandard 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 Deviation = 0.3C.Reproducibility Standard Deviation = 1.4C.14.2.2 For a material hav
46、ing 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 material,method or laboratory for determining the bias for the procedurein these test
47、 methods for measuring the ring-and-ball softeningpoint, no statement on bias can be made.15. Keywords15.1 hydrocarbon resin; ring and ball; rosin based resins;softening pointAPPENDIX(Nonmandatory Information)X1. ALTERNATIVE SAMPLE PREPARATION PROCEDUREX1.1 Preparation of Sample by the Powder Method
48、: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 required:X1.1.2.1 RingAs an alternative to the brass ring conform-i
49、ng 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: sleeve, 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
