ASTM D6090-99
(Test Method)Standard Test Method for Softening Point Resins (Mettler Cup and Ball Method)
Standard Test Method for Softening Point Resins (Mettler Cup and Ball Method)
SCOPE
1.1 This test method covers the determination of softening point of resins using a Mettler cup and ball apparatus, and may, under user defined condition, give results comparable to those obtained by Test Method E 28.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D 6090 – 99
Standard Test Method for
Softening Point Resins (Mettler Cup and Ball Method)
This standard is issued under the fixed designation D 6090; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 5. Apparatus
1.1 This test method covers the determination of softening 5.1 Softening Point Apparatus —This commercially avail-
point of resins using a Mettler cup and ball apparatus, and may, able instrument consists of a control unit with a digital
under user-defined conditions, give results comparable to those temperature indicator; matched measuring cell; cartridge as-
obtained by Test Method E 28. sembly, consisting of a sample cup and upper portion; and
1.2 This standard does not purport to address all of the accessories. The control unit automatically regulates the heat-
safety concerns, if any, associated with its use. It is the ing rate of the measuring cell. The softening point is indicated
responsibility of the user of this standard to establish appro- on the readout, and the heating program stopped, when the
priate safety and health practices and determine the applica- sample flow triggers a photocell detector.
bility of regulatory limitations prior to use. 5.2 Central Processor—This unit shall provide a continu-
ous, linear temperature increase from 25 to 375°C.
2. Referenced Documents
5.3 Measuring Cell— This unit shall be capable of heating
2.1 ASTM Standards:
a sample cup assembly, as described in 5.4, at a linear rate with
E 28 Test Method for Softening Point by Ring-and-Ball an accuracy of 60.2°C/min. It shall include a sensing system
Apparatus
capable of detecting the softening point with a precision of
E 177 Practice for Use of the Terms Precision and Bias in 0.1°C.
ASTM Test Methods
5.4 Sample Cup Assembly—A cup of chromium-plated
E 691 Practice for Conducting an Interlaboratory Study to brass and an upper portion, conforming to the dimensions
Determine the Precision of a Test Method
shown in Fig. 1.
5.5 Ball—A stainless steel ball, 8.7 mm (11/32 in.) in
3. Summary of Test Method
diameter, weighing 2.77 6 0.02 g.
3.1 In this test method, the softening point is defined as the
6. Calibration of Apparatus Using a Primary Standard
temperature at which the sample, suspended in a cylindrical
cup with a 6.35-mm hole in the bottom and with a stainless 6.1 This step, required only occasionally, is designed to
steel ball, 8 mm in diameter, centered on top of the sample in
establish that the temperature indicated by the instrument is in
the cup, flows downward a distance of 19 mm to interrupt a agreement with a known standard. A special cup with a bottom
light beam, as the sample is heated at a linear rate in air.
orifice of 2.8 mm is used instead of the one specified for testing
the resin.
4. Significance and Use
NOTE 1—The stainless steel ball is not used during calibration.
4.1 In general, with materials of these types, softening point
6.2 Reagent—Use either analytical reagent or primary stan-
does not take place at a definite temperature. As the tempera-
dard grade benzoic acid for the calibration. As this material is
ture rises, these materials gradually change from brittle or
hygroscopic, it must be stored in a tightly sealed container, and
exceedingly thick and slow-flowing materials to softer and less
replaced with fresh material from a newly opened supply if
viscous liquids. For this reason, the determination of the
hydration or other contamination is suspected.
softening point must be made by a fixed, arbitrary, and closely
6.3 Procedure:
defined method if the results obtained are to be comparable.
6.3.1 Filling the Sample Cup—Place the cup on a clean, flat
surface and fill it with benzoic acid crystals. Hand press the
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.34 on Naval Stores. The sole source of supply of the apparatus FP90/FP83HT, known to the
Current edition approved June 10, 1999. Published August 1999. Originally
committee at this time is the Mettler-Toledo, Inc., Princeton-Hightstown Rd.,
published as D 6090 – 97. Last previous edition D 6090– 97. Hightstown, NJ 08520. If you are aware of alternative suppliers, please provide this
Annual Book of ASTM Standards, Vol 06.03. information to ASTM Headquarters. Your comments will receive careful consider-
3 1
Annual Book of ASTM Standards, Vol 14.02. ation at a meeting of the resposible technical committee, which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 6090
Table 1. Demonstration of conformance to the dropping point
of benzoic acid should be completed before a secondary
standard is read.
7.2 Follow the same procedure as in 6.3.2 and 6.3.3 but start
about 3°C below the actual dropping point of the secondary
standard.
8. Preparation of Sample
8.1 Fold the tab on an oil-free disposable aluminum weigh-
ing dish to a horizontal position and pinch a pour spout into the
dish directly 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
is almost melted.
8.3 Remove the beaker from the hot plate, grasp the tab with
forceps or needle-nose pliers, and stir the sample with a
probe-type thermometer until it is completely melted and
homogeneous. Avoid entraining air into the sample melt. The
temperature of the sample should be no more than 60°C above
FIG. 1 Specimen Cup
the expected softening point. Remove the thermometer and
wipe clean. If the sample smokes or appears to boil, repeat
material into the cup with a 9.2-mm rod of dowel stock or 8.1-8.3, setting the maximum temperature 10°C less than the
equivalent. Refill and repeat the pressing step until the cup is previous trial.
filled with benzoic acid. Remove any crystals from the exterior 8.4 Filling the Sample Cup:
of the cup. 8.4.1 Arrange two sample cups, small outlet down, on a
6.3.2 Heating—Preheat the measuring cell to 121°C, and
piece of aluminum foil placed on a smooth, flat surface.
maintain it at that temperature. Place the cartridge assembly 8.4.2 Grasping the dish tab with forceps or pliers, pour the
containing the benzoic acid in position in the measuring cell,
molten resin into both of the sample cups. Fill the cups to the
taking care that the slits for the light beam are properly brim without excessive overfilling.
positioned. With the instrument set in the dropping point mode,
8.4.3 Allow the resin to cool for at least 10 min. Cleanly
start the required method, which includes a waiting period of trim off the excess resin on the sample cup with a slightly
30 s to allow temperature equilibration between the measuring
heated knife or spatula, or grasp the cup in a pair of tongs and
cell and s
...
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