ASTM D6090-99(2008)
(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 conditions, give results comparable to those obtained by Test Methods E 28.
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 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.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D6090 − 99 (Reapproved 2008)
StandardTest Method for
Softening Point Resins (Mettler Cup and Ball Method)
This standard is issued under the fixed designation D6090; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope ture rises, these materials gradually change from brittle or
exceedingly thick and slow-flowing materials to softer and less
1.1 This test method covers the determination of softening
viscous liquids. For this reason, the determination of the
point of resins using a Mettler cup and ball apparatus, and may,
softening point must be made by a fixed, arbitrary, and closely
under user-defined conditions, give results comparable to those
defined method if the results obtained are to be comparable.
obtained by Test Methods E28.
1.2 The values stated in SI units are to be regarded as the
5. Apparatus
standard. The values given in parentheses are for information
5.1 Softening Point Apparatus —This commercially avail-
only.
able instrument consists of a control unit with a digital
1.3 This standard does not purport to address all of the
temperature indicator; matched measuring cell; cartridge
safety concerns, if any, associated with its use. It is the
assembly, consisting of a sample cup and upper portion; and
responsibility of the user of this standard to establish appro-
accessories. The control unit automatically regulates the heat-
priate safety and health practices and determine the applica-
ing rate of the measuring cell. The softening point is indicated
bility of regulatory limitations prior to use.
on the readout, and the heating program stopped, when the
sample flow triggers a photocell detector.
2. Referenced Documents
2 5.2 Central Processor—This unit shall provide a
2.1 ASTM Standards:
continuous, linear temperature increase from 25 to 375°C.
E28 Test Methods for Softening Point of Resins Derived
from Naval Stores by Ring-and-Ball Apparatus 5.3 Measuring Cell—This unit shall be capable of heating a
E177 Practice for Use of the Terms Precision and Bias in sample cup assembly, as described in 5.4, at a linear rate with
ASTM Test Methods an accuracy of 60.2°C/min. It shall include a sensing system
E691 Practice for Conducting an Interlaboratory Study to capable of detecting the softening point with a precision of
Determine the Precision of a Test Method 0.1°C.
5.4 SampleCupAssembly—Acupofchromium-platedbrass
3. Summary of Test Method
and an upper portion, conforming to the dimensions shown in
3.1 In this test method, the softening point is defined as the
Fig. 1.
temperature at which the sample, suspended in a cylindrical
5.5 Ball—A stainless steel ball, 8.7 mm ( ⁄32 in.) in
cup with a 6.35-mm hole in the bottom and with a stainless
diameter, weighing 2.77 6 0.02 g.
steel ball, 8 mm in diameter, centered on top of the sample in
the cup, flows downward a distance of 19 mm to interrupt a
6. Calibration of Apparatus Using a Primary Standard
light beam, as the sample is heated at a linear rate in air.
6.1 This step, required only occasionally, is designed to
4. Significance and Use
establish that the temperature indicated by the instrument is in
agreement with a known standard.Aspecial cup with a bottom
4.1 In general, with materials of these types, softening point
orificeof2.8mmisusedinsteadoftheonespecifiedfortesting
does not take place at a definite temperature. As the tempera-
the resin.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
NOTE 1—The stainless steel ball is not used during calibration.
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.34 on Pine Chemicals and Hydrocarbon Resins.
Current edition approved June 1, 2008. Published June 2008. Originally
approved in 1997. Last previous edition approved in 2004 as D6090 – 99 (2004). The sole source of supply of the apparatus FP90/FP83HT, known to the
DOI: 10.1520/D6090-99R08. 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 (Reapproved 2008)
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
FIG. 1 Specimen Cup
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
6.2 Reagent—Use either analytical reagent or primary stan-
is almost melted.
dard grade benzoic acid for the calibration. As this material is
hygroscopic, it must be stored in a tightly sealed container, and
8.3 Removethebeakerfromthehotplate,graspthetabwith
replaced with fresh material from a newly opened supply if
forceps or needle-nose pliers, and stir the sample with a
hydration or other contamination is suspected.
probe-type thermometer until it is completely melted and
homogeneous. Avoid entraining air into the sample melt. The
6.3 Procedure:
temperature of the sample should be no more than 60°C above
6.3.1 Filling the Sample Cup—Place the cup on a clean, flat
the expected softening point. Remove the thermometer and
surface and fill it with benzoic acid crystals. Hand press the
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
of the cup. 8.4 Filling the Sample Cup:
6.3.2 Heating—Preheat the measuring cell to 121°C, and
8.4.1 Arrange two sample cups, small outlet down, on a
maintain it at that temperature. Place the cartridge assembly piece of aluminum foil placed on a smooth, flat surface.
containing the benzoic acid in position in the measuring cell,
8.4.2 Grasping the dish tab with forceps or pliers, pour the
taking care that the slits f
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.