ASTM D6493-99
(Test Method)Standard Test Methods for Softening Point of Hydrocarbon Resins by Automated Ring and Ball Apparatus
Standard Test Methods for Softening Point of Hydrocarbon Resins by Automated Ring and Ball Apparatus
SCOPE
1.1 These test methods are intended for determining the softening point of hydrocarbon resins and similar materials by means of an automated ring-and-ball apparatus.
1.1.1 The ring and ball softening point of a hydrocarbon resin may be run with lower precision using the manual ring and ball softening point in Test Method 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.
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Designation:D6493–99
Standard Test Methods for
Softening Point of Hydrocarbon Resins by Automated Ring
and Ball Apparatus
This standard is issued under the fixed designation D 6493; 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 horizontal ring is forced downward a distance of 25.4 mm (1
in.) under the weight of a steel ball as the sample is heated at
1.1 These test methods are intended for determining the
5°C/mininawater,glycerin,siliconeoil,ethyleneglycol/water
softening point of hydrocarbon resins and similar materials by
or glycerin/water bath.
means of an automated ring-and-ball apparatus.
1.1.1 The ring and ball softening point of a hydrocarbon
4. Sample Preparation
resin may be run with lower precision using the manual ring
4.1 Preparation of Sample by the Pour Method:
and ball softening point in Test MethodE28.
4.1.1 This procedure is suitable for materials that can be
1.2 The values stated in SI units are to be regarded as the
heated and poured without adverse effects on the softening
standard. The values given in parentheses are for information
point.
only.
4.1.2 Select a sample representative of the material to be
1.3 This standard method does not purport to address all of
tested. The sample should consist of flakes, pastilles, or freshly
the safety concerns, if any, associated with its use. It is the
broken lumps. Avoid inclusion of finely divided material or
responsibility of the user of this standard to establish appro-
dust.
priate safety and health practices and determine the applica-
4.1.3 Select a quantity at least twice that necessary to fill the
bility of regulatory limitations prior to use.
desired number of rings, and melt it in a clean container, using
2. Referenced Documents an oven, hot plate, sand bath or oil bath to prevent local
overheating.Take care to avoid incorporating air bubbles in the
2.1 ASTM Standards:
2 sample. Melt the sample completely, but do not heat it above a
E 1 Specification for ASTM Thermometers
temperature necessary to pour the material readily. The time
E28 Test Methods for Softening Point of Resins Derived
from the beginning of heating to the pouring of the sample
from Naval Stores by Ring-and-Ball Apparatus
should not exceed 15 min.
E 177 Practice for Use of the Terms Precision and Bias in
4.1.4 For materials that tend to crack or shrink in the ring on
ASTM Test Methods
cooling, immediately before filling the ring, preheat the ring to
E 691 Practice for Conducting an Interlaboratory Study to
approximately the temperature at which the material is to be
Determine the Precision of a Test Method
poured. The ring, while being filled, should rest bottom down
3. Significance and Use on a suitable metal surface. Pour the sample into the ring so as
to leave an excess on cooling. After cooling a minimum of 30
3.1 In general, with materials of these types, softening does
min, trim off the excess resin on the periphery of the ring. To
not take place at a definite temperature. As the temperature
remove excess resin from the top, cut the excess material off
rises, these materials gradually change from brittle or exceed-
cleanly with a slightly heated knife or spatula, or grasp the ring
ingly thick and slow-flowing materials to softer and less
in a pair of tongs and draw the top surface quickly and firmly
viscous liquids. For this reason, the determination of the
over the surface of a heated metal plate. In case the test is
softening point must be made by a fixed, arbitrary, and closely
repeated, use a clean container and fresh sample.
defined method if the results obtained are to be comparable.
4.2 Preparation of Sample by the Powder Method:
3.2 In these test methods, the softening point is defined as
4.2.1 See Appendix X1.1, Alternate Sample Preparation
the temperature at which a disk of the sample held within a
Procedures.
4.3 Preparation of Samples Having a Low Softening Point
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD-1onPaint
(up to 35°C (95°F)):
and Related Coatings, Materials, and Applications , and is the direct responsibility
4.3.1 Place a ring on a piece of aluminum foil. Pour the
of Subcommittee D01.38 on Hydrocarbon Resins.
Current edition approved Dec. 10, 1999. Published February 2000.
material to be tested into the ring, then place the foil and the
Annual Book of ASTM Standards, Vol 14.03.
filled ring on dry ice or in a freezer to cool. The material in the
Annual Book of ASTM Standards, Vol 06.03.
4 ring must be free of bubbles.
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6493–99
FIG. 1 Shouldered Ring, Ring Holder, Ball-Centering Guide, and Assembly of Apparatus Showing Two Rings
4.3.2 After cooling, cut and scrape off any excess material 6.1.1.1 Use distilled or deionized water that has been cooled
using a slightly heated spatula, then slide the ring gently from to at least 27°C (81°F) below the anticipated softening point,
the foil. Place the ring in the supporting apparatus, and perform but in no case lower than 5°C (41°F).
the softening point analysis according to Section 11. 6.1.2 USP Glycerin—For softening points between 80°C
(176°F) and 150°C (302°F). Repeated use of glycerin will
5. Apparatus
increase the moisture content over time and may affect results.
Replace with fresh glycerin if any change in appearance is
5.1 Automated Ring and Ball Softening Point Instrument
noted.
with Control Unit, test units, and test inserts.
5.2 Ring—A brass, shouldered ring conforming to the
NOTE 1—Glycerin should not be used for softening points greater than
dimensions shown in Fig. 1(a).
150°C (302°F) due to the 160°C (320°F) flash point of glycerin.
5.3 Ball—A steel ball, 9.53 6 0.1 mm ( ⁄8 in.) in diameter,
6.1.3 Silicone Oil (Polydimethylsiloxane)—For softening
weighing between 3.45 and 3.55 g.
points above 80°C (176°F). The oil must have a temperature
5.4 Beaker, 600 mL. Ensure that the dimensions will prop-
rangeof200°C+(392°F+),remainclearwithinthetemperature
erly fit the heating unit.
range, have no apparent effect or reactivity with the test
5.5 Stir Bar—The dimensions must be such that the bar
specimen, have a high water repellency, and maintain a
spins freely under the test stand.
uniform viscosity and stirring rate within the temperature
range.
6. Reagents and Materials
6.1 Bath Liquids:
6.1.1 Distilled or Deionized Water, Freshly Boiled—For
Supporting data are available from ASTM Headquarters. Request
softening points between 35°C (95°F) and 80°C (176°F). RR:D01–1113.
D6493–99
NOTE 2—Replace with fresh silicone oil if any change in appearance is
11. Procedure for Materials Having Softening Points
noted. Do not use silicone oil that contains any gels; gels are an indicator
Below 35°C (95°F)
that degradation has occurred.
11.1 Apparatus:
6.1.4 Ethylene Glycol—For softening points up to 35°C
11.1.1 Isopropyl Alcohol Dry Ice Bath.
(95°F).
11.2 Procedure:
6.1.4.1 Prepare a fresh 50/50 (volume/volume) mixture of
11.2.1 Cool the bath, described in 6.1.4.1, to –25°C (–13°F)
distilledwaterandethyleneglycolpriortosampleanalysis.For
in an isopropyl alcohol dry ice bath.
softening points between 0°C and 35°C, a 50/50 (v/v) mixture
11.2.2 Use the same procedure as in Section 8 except for the
of glycerin and water may be used.
bath liquid, and begin heating as directed once the test
specimen in the ring has been placed in the bath.
7. Calibration
7.1 The calibration of any automated ring and ball softening
12. Report
point apparatus must be performed on a regular basis, since
12.1 Report the
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