1、Designation: D6090 99 (Reapproved 2008) D6090 12Standard Test Method forSoftening Point Resins (Mettler Cup and Ball Method)1This standard is issued under the fixed designation D6090; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、 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. Scope1.1 This test method covers the determination of softening point of resins using a Mettler cup and ball appar
3、atus, and may, underuser-defined conditions, give results comparable to those obtained by Test Methods E28.1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.3 This standard does not purport to address all of the safety co
4、ncerns, 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:2E28 Test Methods for Softening Point of
5、Resins Derived from Naval Stores by Ring-and-Ball ApparatusE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Summary of Test Method3.1 In this test method, the softening point
6、is defined as the temperature at which the sample, suspended in a cylindrical cupwith a 6.35-mm hole in the bottom and with a stainless steel ball, 8 mm in diameter, centered on top of the sample in the cup, flowsdownward a distance of 19 mm to interrupt a light beam, as the sample is heated at a li
7、near rate in air.4. Significance and Use4.1 In general, with materials of these types, softening point does not take place at a definite temperature. As the temperaturerises, these materials gradually change from brittle or exceedingly thick and slow-flowing materials to softer and less viscousliqui
8、ds. For this reason, the determination of the softening point must be made by a fixed, arbitrary, and closely defined methodif the results obtained are to be comparable.5. Apparatus5.1 Softening Point Apparatus3This commercially available instrument consists of a control unit with a digital temperat
9、ureindicator; matched measuring cell; cartridge assembly, consisting of a sample cup and upper portion; and accessories. The controlunit automatically regulates the heating rate of the measuring cell. The softening point is indicated on the readout, and the heatingprogram stopped, when the sample fl
10、ow triggers a photocell detector.5.2 Central ProcessorThis unit shall provide a continuous, linear temperature increase from 25 to 375C.5.3 Measuring CellThis unit shall be capable of heating a sample cup assembly, as described in 5.4, at a linear rate with anaccuracy of 60.2C/min. It shall include
11、a sensing system capable of detecting the softening point with a precision of 0.1C.1 This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.34 on Pine Chemicals and Hydrocarbon Re
12、sins.Current edition approved June 1, 2008Nov. 1, 2012. Published June 2008December 2012. Originally approved in 1997. Last previous edition approved in 20042008 asD6090 99 (2004).(2008). DOI: 10.1520/D6090-99R08.10.1520/D6090-12.2 For referenced ASTM standards, visit the ASTM website, www.astm.org,
13、 or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The sole source of supply of the apparatus FP90/FP83HT, known to the committee at this time is the Mettler-Toledo, Inc., Princ
14、eton-Hightstown Rd., Hightstown, NJ08520. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration ata meeting of the responsible technical committee,1 which you may attend.This document is not an
15、ASTM standard and is intended only to provide the user of an ASTM 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
16、 all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.4 Sample Cup AssemblyA cup of chromium-plated brass and an upper porti
17、on, conforming to the dimensions shown in Fig.1.5.5 BallA stainless steel ball, 8.7 mm (1132 in.) in diameter, weighing 2.77 6 0.02 g.6. Calibration of Apparatus Using a Primary Standard6.1 This step, required only occasionally, is designed to establish that the temperature indicated by the instrume
18、nt is inagreement with a known standard. A special cup with a bottom orifice of 2.8 mm is used instead of the one specified for testingthe resin.NOTE 1The stainless steel ball is not used during calibration.6.2 ReagentUse either analytical reagent or primary standard grade benzoic acid for the calib
19、ration. As this material ishygroscopic, it must be stored in a tightly sealed container, and 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, flat surface and fill it with benzo
20、ic acid crystals. Hand press the materialinto the cup with a 9.2-mm rod of dowel stock or equivalent. Refill and repeat the pressing step until the cup is filled with benzoicacid. Remove any crystals from the exterior of the cup.6.3.2 HeatingPreheat the measuring cell to 121C, and maintain it at tha
21、t temperature. Place the cartridge assembly containingthe benzoic acid in position in the measuring cell, taking care that the slits for the light beam are properly positioned. With theinstrument set in the dropping point mode, start the required method, which includes a waiting period of 30 s to al
22、low temperatureequilibration between the measuring cell and sample followed by an automatic temperature ramp of 0.2C/min. The temperaturewill rise steadily at the correct rate until the drop point is reached, and then remain steady on the readout.6.3.3 CleaningImmediately remove the cartridge assemb
23、ly. Check to determine that the sample has passed through the lightbeam and no pre-triggering has occurred. If a malfunction is suspected, the entire procedure must be repeated. Inspect the apparatuscarefully to ensure that no residue remains. Wash the cartridge parts with a suitable solvent to remo
24、ve the last traces of 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 the acceptablerange, repeat the test using a fresh sample of benzoic acid. If the results remain outside of the acceptable range, the instrumentrequires re
25、calibration or repair. Consult the manufacturers instruction manual.7. Instrument Check of Apparatus Using a Secondary Standard7.1 The primary calibration standard, benzoic acid, might not have a dropping point similar to the softening point of the resinbeing tested. In such cases, it is desirable t
26、o calibrate the instrument using a secondary standard having a dropping point similarto that of the test sample. Materials suitable for use as secondary standards are listed, but are not limited to those, in Table 1.Demonstration of conformance to the dropping point of benzoic acid should be complet
27、ed before a secondary standard is read.7.2 Follow the same procedure as in 6.3.2 and 6.3.3 but start about 3C below the actual dropping point of the secondarystandard.FIG. 1 Specimen CupD6090 1228. Preparation of Sample8.1 Fold the tab on an oil-free disposable aluminum weighing dish to a horizontal
28、 position and pinch a pour spout into the dishdirectly opposite the tab. Weigh 5 to 10 g of resin into the dish.8.2 Place the dish and sample on a preheated hot plate and cover with a 600-mL or larger beaker. Heat the sample until it isalmost melted.8.3 Remove the beaker from the hot plate, grasp th
29、e tab with forceps or needle-nose pliers, and stir the sample with a probe-typethermometer until it is completely melted and homogeneous. Avoid entraining air into the sample melt. The temperature of thesample should be no more than 60C above the expected softening point. Remove the thermometer and
30、wipe clean. If the samplesmokes or appears to boil, repeat 8.1-8.3, setting the maximum temperature 10C less than the previous trial.8.4 Filling the Sample Cup:8.4.1 Arrange two sample cups, small outlet down, on a piece of aluminum foil placed on a smooth, flat surface.8.4.2 Grasping the dish tab w
31、ith forceps or pliers, pour the molten resin into both of the sample cups. Fill the cups to the brimwithout excessive overfilling.8.4.3 Allow the resin to cool for at least 10 min. Cleanly trim off the excess resin on the sample cup with a slightly heated knifeor spatula, or grasp the cup in a pair
32、of tongs and draw the top surface quickly and firmly over the surface of a heated metal plate.Do not make a determination on a sample that contains air bubbles.8.4.4 Assemble the cartridge by placing the cup on the collector, then the upper portion on the cup. Carefully place the ball ontop of the c
33、up.8.4.5 Make sure that there is no sample on the outside of the cup, the inside of the jacket, or the collecting sleeve. Thesecomponents must be clean during analysis. The assembly should be wiped clean before inserting it into the measuring.9. Procedure9.1 The procedure described is for measuring
34、the Mettler cup and ball softening point of resins. The heating rate is usuallydetermined by the user. Heating rates of 1.0 to 2.5C/min are typical for resins. If a correlation is desired between Mettler cup andball softening point and ring-and-ball softening point as described in Test Methods E28,
35、a specific heating rate for that correlationmust be determined for each type of resin.NOTE 2To facilitate a comparison of Mettler cup and ball softening point results between laboratories, a reference set of conditions is provided asfollows:Cup: 6.35-mm diameter.Heating Rate: 1.6C/min.Starting Tempe
36、rature: 20C below the expected softening point of the resin.9.2 Preset the starting temperature of the central processor from 20 to 25C below the expected softening point of the sampleand maintain this temperature for a few minutes. Assemble the cartridge with the stainless steel ball carefully cent
37、ered on top ofthe sample. Place the cartridge assembly in the measuring cell, taking care that the slits for the light beam are properly positioned.With the instrument in the softening point mode, start the determination, which includes a waiting period of 30 s to allowtemperature equilibration betw
38、een the measuring cell and sample followed by automatic temperature ramp at the specified rate inC/min. Heating will be maintained at this rate until the drop point is reached, after which a steady temperature still be displayedon the readout. Record this temperature as the softening point of the sa
39、mple.9.3 Remove the cartridge assembly upon completion of the test. Check to ensure that the sample has passed through the lightbeam and no pre-triggering has occurred. If a malfunction is suspected, reject the result and repeat the test. Inspect the apparatusclosely to ensure that no particles of r
40、esidue remain.TABLE 1 Materials Suitable as Secondary Standards for MettlerCup and Ball Softening PointApproximate Dropping Point,CPoint, CMaterial60 stearyl alcohol80 diphenyl carbonatenaphthalene100 phenoxyacetic acid4-t-butylphenolmethyl urea110 m-toluic acidresorcinol120 benzoic acid130 methyl 4
41、-hydroxybenzoateureabenzamide1,10-decanedicarboxylic acid140 dimethyl terephthalateo-toluamideD6090 1239.4 Clean the sample cup and ball by soaking in a suitable solvent.NOTE 3Care must be taken in cleaning the sample cup in order not to scratch or alter the size of the cup orifice.9.5 Clean the int
42、erior of the cell immediately after removing the 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 interlabor
43、atory precision study was conducted using the same materials asthat reported in Test Methods E28.11.2 An interlaboratory study of the Mettler cup and ball softening point of three hydrocarbon resins was conducted in 1998,in accordance with Practice E691, by 10 laboratories. The test conditions were
44、those listed in Note 2. The precision informationgiven as follows is for the comparison of two test results.11.3 Precision:11.3.1 Repeatability Limit, 95 % (within laboratory) ;0.5 to 1.3C.11.3.2 Reproducibility Limit, 95 % (between laboratories) ;1.4 to 2.1C.11.3.3 The above terms (repeatability li
45、mit and reproducibility limit) are used in accordance with Practice E177. The respectivestandard deviations among test results, related to the preceding 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
46、 BiasSince there is no accepted reference material, method, or laboratory suitable for determining the bias for theprocedure in this test method for measuring softening point, no statement on bias is being made.12. Keywords12.1 resin; softening pointASTM International takes no position respecting th
47、e 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 standard i
48、s 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 International He
49、adquarters. 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 below.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 aboveaddres
