ASTM D6090-99(2004)
(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)
SIGNIFICANCE AND USE
In general, with materials of these types, softening point does not take place at a definite temperature. As the temperature rises, these materials gradually change from brittle or exceedingly thick and slow-flowing materials to softer and less viscous liquids. For this reason, the determination of the softening point must be made by a fixed, arbitrary, and closely defined method if the results obtained are to be comparable.
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:D6090–99(Reapproved2004)
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 exceedingly thick and slow-flowing materials to softer and less
viscous liquids. For this reason, the determination of the
1.1 This test method covers the determination of softening
softening point must be made by a fixed, arbitrary, and closely
point of resins using a Mettler cup and ball apparatus, and may,
defined method if the results obtained are to be comparable.
under user-defined conditions, give results comparable to those
obtained by Test Methods E 28.
5. Apparatus
1.2 The values stated in SI units are to be regarded as the
5.1 Softening Point Apparatus —This commercially avail-
standard. The values given in parentheses are for information
able instrument consists of a control unit with a digital
only.
temperature indicator; matched measuring cell; cartridge as-
1.3 This standard does not purport to address all of the
sembly, consisting of a sample cup and upper portion; and
safety concerns, if any, associated with its use. It is the
accessories. The control unit automatically regulates the heat-
responsibility of the user of this standard to establish appro-
ing rate of the measuring cell. The softening point is indicated
priate safety and health practices and determine the applica-
on the readout, and the heating program stopped, when the
bility of regulatory limitations prior to use.
sample flow triggers a photocell detector.
2. Referenced Documents 5.2 Central Processor—This unit shall provide a continu-
ous, linear temperature increase from 25 to 375°C.
2.1 ASTM Standards:
5.3 Measuring Cell— This unit shall be capable of heating
E 28 Test Methods for Softening Point of Resins Derived
a sample cup assembly, as described in 5.4, at a linear rate with
from Naval Stores by Ring-and-Ball Apparatus
an accuracy of 60.2°C/min. It shall include a sensing system
E 177 Practice for Use of the Terms Precision and Bias in
capable of detecting the softening point with a precision of
ASTM Test Methods
0.1°C.
E 691 Practice for Conducting an Interlaboratory Study to
5.4 Sample Cup Assembly—A cup of chromium-plated
Determine the Precision of a Test Method
brass and an upper portion, conforming to the dimensions
3. Summary of Test Method shown in Fig. 1.
5.5 Ball—A stainless steel ball, 8.7 mm ( ⁄32 in.) in
3.1 In this test method, the softening point is defined as the
diameter, weighing 2.77 6 0.02 g.
temperature at which the sample, suspended in a cylindrical
cup with a 6.35-mm hole in the bottom and with a stainless
6. Calibration of Apparatus Using a Primary Standard
steel ball, 8 mm in diameter, centered on top of the sample in
6.1 This step, required only occasionally, is designed to
the cup, flows downward a distance of 19 mm to interrupt a
establish that the temperature indicated by the instrument is in
light beam, as the sample is heated at a linear rate in air.
agreement with a known standard.Aspecial cup with a bottom
4. Significance and Use
orificeof2.8mmisusedinsteadoftheonespecifiedfortesting
the resin.
4.1 In general, with materials of these types, softening point
does not take place at a definite temperature. As the tempera-
NOTE 1—The stainless steel ball is not used during calibration.
ture rises, these materials gradually change from brittle or
6.2 Reagent—Use either analytical reagent or primary stan-
dard grade benzoic acid for the calibration. As this material is
hygroscopic, it must be stored in a tightly sealed container, and
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.34 on Naval Stores.
CurrenteditionapprovedJune1,2004.PublishedJuly2004.Originallyapproved The sole source of supply of the apparatus FP90/FP83HT, known to the
in 1997. Last previous edition approved in 1999 as D 6090 – 99. committee at this time is the Mettler-Toledo, Inc., Princeton-Hightstown Rd.,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Hightstown, NJ 08520. If you are aware of alternative suppliers, please provide this
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM information to ASTM International Headquarters. Your comments will receive
Standards volume information, refer to the standard’s Document Summary page on careful consideration at a meeting of the responsible technical committee, which
the ASTM website. you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6090–99 (2004)
7. Instrument Check of Apparatus Using a Secondary
Standard
7.1 The primary calibration standard, benzoic acid, might
not have a dropping point similar to the softening point of the
resin being tested. In such cases, it is desirable to calibrate the
instrument using a secondary standard having a dropping point
similar to 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 completed before a secondary
standard is read.
7.2 Followthesameprocedureasin6.3.2and6.3.3butstart
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.
FIG. 1 Specimen Cup
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.
replaced with fresh material from a newly opened supply if
8.3 Removethebeakerfromthehotplate,graspthetabwith
hydration or other contamination is suspected.
forceps or needle-nose pliers, and stir the sample with a
6.3 Procedure:
probe-type thermometer until it is completely melted and
6.3.1 Filling the Sample Cup—Place the cup on a clean, flat
homogeneous. Avoid entraining air into the sample melt. The
surface and fill it with benzoic acid crystals. Hand press the
temperature of the sample should be no more than 60°C above
material into the cup with a 9.2-mm rod of dowel stock or
the expected softening point. Remove the thermometer and
equivalent. Refill and repeat the pressing step until the cup is
wipe clean. If the sample smokes or appears to boil, repeat
filled with benzoic acid. Remove any crystals from the exterior
8.1-8.3, setting the maximum temperature 10°C less than the
of the cup.
previous trial.
6.3.2 Heating—Preheat the measuring cell to 121°C, and 8.4 Filling the Sample Cup:
maintain it at that temperature. Place the cartridge assembly 8.4.1 Arrange two sample cups, small outlet down, on a
containing the benzoic acid in position in the measuring cell, piece of aluminum foil placed on a smooth, flat surface.
taking care that
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