1、Designation: D 6090 99 (Reapproved 2008)Standard Test Method forSoftening Point Resins (Mettler Cup and Ball Method)1This standard is issued under the fixed designation D 6090; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye
2、ar 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. Scope1.1 This test method covers the determination of softeningpoint of resins using a Mettler cup and ball apparatus, an
3、d may,under user-defined conditions, give results comparable to thoseobtained by 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 does not purport to address all of thesafety concerns, if a
4、ny, 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:2E28 Test Methods for Softening Point of Resins De
5、rivedfrom Naval Stores by Ring-and-Ball ApparatusE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Summary of Test Method3.1 In this test method, the softening point is defined
6、 as thetemperature at which the sample, suspended in a cylindricalcup with a 6.35-mm hole in the bottom and with a stainlesssteel ball, 8 mm in diameter, centered on top of the sample inthe cup, flows downward a distance of 19 mm to interrupt alight beam, as the sample is heated at a linear rate in
7、air.4. Significance and Use4.1 In general, with materials of these types, softening pointdoes not take place at a definite temperature. As the tempera-ture rises, these materials gradually change from brittle orexceedingly thick and slow-flowing materials to softer and lessviscous liquids. For this
8、reason, the determination of thesoftening point must be made by a fixed, arbitrary, and closelydefined method if the results obtained are to be comparable.5. Apparatus5.1 Softening Point Apparatus3This commercially avail-able instrument consists of a control unit with a digitaltemperature indicator;
9、 matched measuring cell; cartridge as-sembly, consisting of a sample cup and upper portion; andaccessories. The control unit automatically regulates the heat-ing rate of the measuring cell. The softening point is indicatedon the readout, and the heating program stopped, when thesample flow triggers
10、a photocell detector.5.2 Central ProcessorThis unit shall provide a continu-ous, linear temperature increase from 25 to 375C.5.3 Measuring Cell This unit shall be capable of heatinga sample cup assembly, as described in 5.4, at a linear rate withan accuracy of 60.2C/min. It shall include a sensing s
11、ystemcapable of detecting the softening point with a precision of0.1C.5.4 Sample Cup AssemblyA cup of chromium-platedbrass and an upper portion, conforming to the dimensionsshown in Fig. 1.5.5 BallA stainless steel ball, 8.7 mm (1132 in.) indiameter, weighing 2.77 6 0.02 g.6. Calibration of Apparatu
12、s Using a Primary Standard6.1 This step, required only occasionally, is designed toestablish that the temperature indicated by the instrument is inagreement with a known standard. A special cup with a bottomorifice of 2.8 mm is used instead of the one specified for testingthe resin.NOTE 1The stainle
13、ss steel ball is not used during calibration.6.2 ReagentUse either analytical reagent or primary stan-dard grade benzoic acid for the calibration. As this material ishygroscopic, it must be stored in a tightly sealed container, and1This test method is under the jurisdiction of ASTM Committee D01 on
14、Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.34 on Naval Stores.Current edition approved June 1, 2008. Published June 2008. Originallyapproved in 1997. Last previous edition approved in 2004 as D 6090 99 (2004).2For referenced ASTM standa
15、rds, 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.3The sole source of supply of the apparatus FP90/FP83HT, known to thecommittee at this t
16、ime is the Mettler-Toledo, Inc., Princeton-Hightstown Rd.,Hightstown, NJ 08520. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou
17、may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.replaced with fresh material from a newly opened supply ifhydration or other contamination is suspected.6.3 Procedure:6.3.1 Filling the Sample CupPlace the cup on a clean, fl
18、atsurface and fill it with benzoic acid crystals. Hand press thematerial into the cup with a 9.2-mm rod of dowel stock orequivalent. Refill and repeat the pressing step until the cup isfilled with benzoic acid. Remove any crystals from the exteriorof the cup.6.3.2 HeatingPreheat the measuring cell t
19、o 121C, andmaintain it at that temperature. Place the cartridge assemblycontaining the benzoic acid in position in the measuring cell,taking care that the slits for the light beam are properlypositioned. With the instrument set in the dropping point mode,start the required method, which includes a w
20、aiting period of30 s to allow temperature equilibration between the measuringcell and sample followed by an automatic temperature ramp of0.2C/min. The temperature will rise steadily at the correct rateuntil the drop point is reached, and then remain steady on thereadout.6.3.3 CleaningImmediately rem
21、ove the cartridge assem-bly. Check to determine that the sample has passed through thelight beam and no pre-triggering has occurred. If a malfunctionis suspected, the entire procedure must be repeated. Inspect theapparatus carefully to ensure that no residue remains. Wash thecartridge parts with a s
22、uitable solvent to remove the last tracesof the residue.6.3.4 InterpretationIf the result is not 123.5 6 0.5C,repeat the test. If the second value remains outside of theacceptable range, repeat the test using a fresh sample ofbenzoic acid. If the results remain outside of the acceptablerange, the in
23、strument requires recalibration or repair. Consultthe manufacturers instruction manual.7. Instrument Check of Apparatus Using a SecondaryStandard7.1 The primary calibration standard, benzoic acid, mightnot have a dropping point similar to the softening point of theresin being tested. In such cases,
24、it is desirable to calibrate theinstrument using a secondary standard having a dropping pointsimilar to that of the test sample. Materials suitable for use assecondary standards are listed, but are not limited to those, inTable 1. Demonstration of conformance to the dropping pointof benzoic acid sho
25、uld be completed before a secondarystandard is read.7.2 Follow the same procedure as in 6.3.2 and 6.3.3 but startabout 3C below the actual dropping point of the secondarystandard.8. Preparation of Sample8.1 Fold the tab on an oil-free disposable aluminum weigh-ing dish to a horizontal position and p
26、inch a pour spout into thedish directly opposite the tab. Weigh 5 to 10 g of resin into thedish.8.2 Place the dish and sample on a preheated hot plate andcover with a 600-mL or larger beaker. Heat the sample until itis almost melted.8.3 Remove the beaker from the hot plate, grasp the tab withforceps
27、 or needle-nose pliers, and stir the sample with aprobe-type thermometer until it is completely melted andhomogeneous. Avoid entraining air into the sample melt. Thetemperature of the sample should be no more than 60C abovethe expected softening point. Remove the thermometer andwipe clean. If the sa
28、mple smokes or appears to boil, repeat8.1-8.3, setting the maximum temperature 10C less than theprevious trial.8.4 Filling the Sample Cup:8.4.1 Arrange two sample cups, small outlet down, on apiece of aluminum foil placed on a smooth, flat surface.8.4.2 Grasping the dish tab with forceps or pliers,
29、pour themolten resin into both of the sample cups. Fill the cups to thebrim without excessive overfilling.8.4.3 Allow the resin to cool for at least 10 min. Cleanlytrim off the excess resin on the sample cup with a slightlyFIG. 1 Specimen CupTABLE 1 Materials Suitable as Secondary Standards for Mett
30、lerCup and Ball Softening PointApproximate Dropping Point, C Material60 stearyl alcohol80 diphenyl carbonatenaphthalene100 phenoxyacetic acid4-t-butylphenolmethyl urea110 m-toluic acidresorcinol120 benzoic acid130 methyl 4-hydroxybenzoateureabenzamide1,10-decanedicarboxylic acid140 dimethyl terephth
31、alateo-toluamideD 6090 99 (2008)2heated knife or spatula, or grasp the cup in a pair of tongs anddraw the top surface quickly and firmly over the surface of aheated metal plate. Do not make a determination on a samplethat contains air bubbles.8.4.4 Assemble the cartridge by placing the cup on thecol
32、lector, then the upper portion on the cup. Carefully place theball on top of the cup.8.4.5 Make sure that there is no sample on the outside of thecup, the inside of the jacket, or the collecting sleeve. Thesecomponents must be clean during analysis. The assemblyshould be wiped clean before inserting
33、 it into the measuring.9. Procedure9.1 The procedure described is for measuring the Mettlercup and ball softening point of resins. The heating rate isusually determined by the user. Heating rates of 1.0 to2.5C/min are typical for resins. If a correlation is desiredbetween Mettler cup and ball soften
34、ing point and ring-and-ballsoftening point as described in Test Methods E28, a specificheating rate for that correlation must be determined for eachtype of resin.NOTE 2To facilitate a comparison of Mettler cup and ball softeningpoint results between laboratories, a reference set of conditions isprov
35、ided as follows:Cup: 6.35-mm diameter.Heating Rate: 1.6C/min.Starting Temperature: 20C below the expected softening point of theresin.9.2 Preset the starting temperature of the central processorfrom 20 to 25C below the expected softening point of thesample and maintain this temperature for a few min
36、utes.Assemble the cartridge with the stainless steel ball carefullycentered on top of the sample. Place the cartridge assembly inthe measuring cell, taking care that the slits for the light beamare properly positioned. With the instrument in the softeningpoint mode, start the determination, which in
37、cludes a waitingperiod of 30 s to allow temperature equilibration between themeasuring cell and sample followed by automatic temperatureramp at the specified rate in C/min. Heating will be main-tained at this rate until the drop point is reached, after which asteady temperature still be displayed on
38、 the readout. Recordthis temperature as the softening point of the sample.9.3 Remove the cartridge assembly upon completion of thetest. Check to ensure that the sample has passed through thelight beam and no pre-triggering has occurred. If a malfunctionis suspected, reject the result and repeat the
39、test. Inspect theapparatus closely to ensure that no particles of residue remain.9.4 Clean the sample cup and ball by soaking in a suitablesolvent.NOTE 3Care must be taken in cleaning the sample cup in order not toscratch or alter the size of the cup orifice.9.5 Clean the interior of the cell immedi
40、ately after removingthe sample assembly. Use soft cotton swabs moistened in anappropriate solvent.10. Report10.1 Report the softening point, as indicated by the readout,to the nearest 1.0C.11. Precision and Bias411.1 A limited Mettler cup and ball softening point inter-laboratory precision study was
41、 conducted using the samematerials as that reported in Test Methods E28.11.2 An interlaboratory study of the Mettler cup and ballsoftening point of three hydrocarbon resins was conducted in1998, in accordance with Practice E 691, by 10 laboratories.The test conditions were those listed in Note 2. Th
42、e precisioninformation given as follows is for the comparison of two testresults.11.3 Precision:11.3.1 Repeatability Limit, 95 % (within laboratory) ;0.5 to1.3C.11.3.2 Reproducibility Limit, 95 % (between laboratories);1.4 to 2.1C.11.3.3 The above terms (repeatability limit and reproduc-ibility limi
43、t) are used in accordance with Practice E 177. Therespective standard deviations among test results, related to thepreceding numbers by a factor of 2.8 are:11.3.3.1 Repeatability standard deviation ;0.2 to 0.5C.11.3.3.2 Reproducibility standard deviation ;0.5 to 0.8C.11.4 BiasSince there is no accep
44、ted reference material,method, or laboratory suitable for determining the bias for theprocedure in this test method for measuring softening point, nostatement on bias is being made.12. Keywords12.1 resin; softening pointASTM International takes no position respecting the validity of any patent right
45、s 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 standard is subject to revision at any t
46、ime 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 International Headquarters. Your comments will
47、 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 below.This standard is copyrighted by ASTM
48、 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).4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D011112.D 6090 99 (2008)3
