This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: E28 − 18

Standard Test Methods for

Softening Point of Resins Derived from Pine Chemicals and
Hydrocarbons, by Ring-and-Ball Apparatus1
This standard is issued under the fixed designation E28; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope ASTM Test Methods

1.1 These test methods are intended for determining the E691 Practice for Conducting an Interlaboratory Study to
softening point of resins (including rosin and terpene resins) Determine the Precision of a Test Method
and similar materials by means of the ring-and-ball apparatus. 3. Significance and Use
NOTE 1—For testing asphalts, tars, and pitches, see Test Method D36. 3.1 In general, with materials of these types, softening does
1.1.1 Test method using the automated ring and ball soften- not take place at a definite temperature. As the temperature
ing point apparatus is the reference method and the test method rises, these materials gradually change from brittle or exceed-
using the manual ring and ball method is an alternative method. ingly thick and slow-flowing materials to softer and less
1.2 The values stated in SI units are to be regarded as the viscous liquids. For this reason, the determination of the
standard. The values given in parentheses are for information softening point must be made by a fixed, arbitrary, and closely
only. defined method if the results obtained are to be comparable.
1.3 This standard does not purport to address all of the 3.2 In these test methods, the softening point is defined as
safety concerns, if any, associated with its use. It is the the temperature at which a disk of the sample held within a
responsibility of the user of this standard to establish appro- horizontal ring is forced downward a distance of 25.4 mm
priate safety, health, and environmental practices and deter- (1 in.) under the weight of a steel ball as the sample is heated
mine the applicability of regulatory limitations prior to use. at 5°C/min in a water, glycerin, silicone oil, ethylene glycol/
1.4 This international standard was developed in accor- water or glycerin/water bath.
dance with internationally recognized principles on standard- 3.3 The automatic method was chosen to be the reference
ization established in the Decision on Principles for the method because a round robin demonstrated that it gave more
Development of International Standards, Guides and Recom- precise results than the manual method.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 4. Sample Preparation
4.1 Preparation of Sample by the Pour Method:
2. Referenced Documents 4.1.1 This procedure is suitable for materials that can be
2.1 ASTM Standards:2 heated and poured without adverse effects on the softening
D36 Test Method for Softening Point of Bitumen (Ring-and- point.
Ball Apparatus) 4.1.2 Select a sample representative of the material to be
E1 Specification for ASTM Liquid-in-Glass Thermometers tested. The sample should consist of flakes, pastilles, or freshly
E177 Practice for Use of the Terms Precision and Bias in broken lumps free of oxidized surfaces. Avoid inclusion of
finely divided material or dust.
4.1.3 Select a quantity at least twice that necessary to fill the
1
These test methods are under the jurisdiction of ASTM Committee D01 on desired number of rings, and melt it immediately in a clean
Paint and Related Coatings, Materials, and Applications and are the direct container, using an oven, hot plate, sand bath or oil bath to
responsibility of Subcommittee D01.34 on Pine Chemicals and Hydrocarbon
Resins.
prevent local overheating. Take care to avoid incorporating air
Current edition approved July 1, 2018. Published July 2018. Originally approved bubbles in the sample. Melt the sample completely, but do not
in 1936. Last previous edition approved in 2014 as E28 – 14. DOI: 10.1520/E0028- heat it above a temperature necessary to pour the material
18. readily. The time from the beginning of heating to the pouring
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM of the sample should not exceed 15 min.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 E28 − 18
NOTE 2—For materials that may be heat sensitive, continuously inert 6.2 Ring—A brass, shouldered ring conforming to the di-
the flask containing the test specimen with nitrogen (N2) during the mensions shown in Fig. 1(a).
remelting procedure.
4.1.4 For materials that tend to crack or shrink in the ring on 6.3 Ball—A steel ball, 9.53 6 0.1 mm (3⁄8 in.) in diameter,
cooling, immediately before filling the ring, preheat the ring to weighing between 3.45 and 3.55 g.
approximately the temperature at which the material is to be 6.4 Beaker, 600 mL or what is recommended by the manu-
poured. The ring, while being filled, should rest bottom down facturer. Ensure that the dimensions will properly fit the
on a suitable metal surface. Pour the sample into the ring so as heating unit.
to leave an excess on cooling. After cooling a minimum of 30
min, trim off the excess resin on the periphery of the ring. To 6.5 Stir Bar—The dimensions must be such that the bar
remove excess resin from the top, cut the excess material off spins freely under the test stand. It is recommended that the
cleanly with a slightly heated knife or spatula, or grasp the ring stirring bar supplied with the instrument be used or one that has
in a pair of tongs and draw the top surface quickly and firmly been shown to give the same result as the one supplied.
over the surface of a heated metal plate. In case the test is
repeated, use a clean container and fresh sample. 7. Procedure for Materials Having a Softening Point
Between 35°C (95°F) and <80°C (176°F)
5. Reagents and Materials
7.1 Add a stir bar to the 600–mL beaker and fill with
5.1 Bath Liquids: approximately 500 mL of distilled or deionized water, con-
5.1.1 Distilled or Deionized Water, Freshly Boiled—For forming to the requirements in 5.1.1. Ensure that the beaker is
softening points between 35°C (95°F) and 80°C (176°F). properly positioned on the heater in the test unit. Place the
5.1.1.1 Use distilled or deionized water that has been cooled prepared sample rings in the test insert. Place the ball-centering
to at least 27°C (81°F) below the anticipated softening point, guide and ball on top of the sample ring. Place the test insert in
but in no case lower than 5°C (41°F). the beaker of water, suspending it from the support pins. Place
5.1.2 USP Glycerin—For softening points between 80°C the temperature measuring device in the test insert. Verify that
(176°F) and 150°C (302°F). Repeated use of glycerin will the control unit is set for the correct bath liquid.
increase the moisture content over time and may affect results.
Replace with fresh glycerin if any change in appearance is 7.2 Heating—Heat the bath so that the temperature of the
noted. water is raised uniformly at a rate of 5°C (10°F)/min. Protect
the bath from drafts, using shields if necessary. The maximum
NOTE 3—Glycerin should not be used for softening points greater than
150°C (302°F) due to the 160°C (320°F) flash point of glycerin.
permissible variation for any one min. period after the first
three min. is 60.5°C (61°F). Reject any test in which the rate
5.1.3 Silicone Oil (Polydimethylsiloxane)—For softening of temperature rise does not fall within these limits. The test is
points above 80°C (176°F). The silicone oil must have a complete when the light beam has been interrupted by the
temperature range of 200°C + (392°F), remain clear within the falling ball and material.
temperature range, have no apparent reactivity with the test
specimen, have a high water repellency, and maintain a NOTE 5—Rigid adherence to the prescribed rate of heating is absolutely
uniform viscosity and stirring rate within the temperature essential for reproducibility of results.
range.3 7.3 Softening Point—Record as the softening point the
NOTE 4—Replace with fresh silicone oil if any change in appearance is temperature displayed on the unit after the light beam has been
noted. Do not use silicone oil that contains any gels; gels are an indicator interrupted by the falling ball and material.
that degradation has occurred.
7.4 Start the cooling process in the instrument. Remove the
5.1.4 Ethylene Glycol/Water—For softening points up to temperature measuring device from the test insert, then remove
35°C (95°F). the test insert from the beakers. Thoroughly clean the test
5.1.4.1 Prepare a fresh 50/50 (v/v) mixture of distilled water insert, ball, and ring in a suitable solvent.
and ethylene glycol prior to sample analysis. For softening
points between 0°C and 35°C, a 50/50 (v/v) mixture of glycerin
8. Calibration
and water may be used.
8.1 The calibration of any automated ring and ball-softening
REFERENCE METHOD point apparatus must be performed on a regular basis since
AUTOMATED RING AND BALL SOFTENING POINT accurate temperature control is required. Follow the manufac-
METHOD turer’s instructions for calibration of the instrument.
6. Apparatus
9. Procedure for Materials Having Softening Points
6.1 Automated Ring and Ball-Softening Point Instrument
Between 80°C (176°F) and 150°C (302°F)
with Control Unit, test units, and test inserts.
9.1 Use the same procedure as described in Section 7,
3
The sole source of supply of silicone oil, 200 fluid, 50 cSt viscosity known to except fill the bath with glycerin or silicone oil.
the committee at this time is Dow Corning Corp., Midland, MI 48686. If you are
aware of alternative suppliers, please provide this information to ASTM Interna- NOTE 6—For materials softening around 80°C (176°F), report the bath
tional Headquarters. Your comments will receive careful consideration at a meeting liquid since a glycerin or silicone oil bath will yield a slightly higher result
of the responsible technical committee,1 which you may attend. than a water bath.

2
 E28 − 18

FIG. 1 Shouldered Ring, Ring Holder, Ball-Centering Guide, and Assembly of Apparatus Showing Two Rings

10. Procedure for Materials Having Softening Points ALTERNATE METHOD

Above 150°C (302°F) MANUAL RING AND BALL SOFTENING POINT
10.1 Use the same procedure as described in Section 7, METHOD
except fill the bath with silicone oil (Note 3).
13. Apparatus
11. Procedure for Materials Having Softening Points 13.1 Ring and Ball Apparatus, consisting of the following:
Below 35°C (95°F) 13.1.1 Ring—A brass, shouldered ring conforming to the
11.1 Apparatus: dimensions shown in Fig. 1(a).
11.1.1 Freezer or Isopropyl Alcohol Dry-Ice Bath. 13.1.2 Ball—A steel ball, 9.53 6 0.1 mm (3⁄8 in.) in
diameter, weighing between 3.45 and 3.55 g.
11.2 Procedure: 13.1.3 Ball-Centering Guide—A brass guide for centering
11.2.1 Cool the bath, described in 5.1.4.1, to −25°C (−13°F) the ball conforming to the general shape and dimensions shown
in the precooled freezer or an isopropyl alcohol dry-ice bath. in Fig. 1(c), the use of which is optional.
11.2.2 Use the same procedure as in Section 7. Take care to
immediately begin heating as directed once the test specimen 13.2 Support for Ring and Thermometer—Any convenient
in the ring has been placed in the bath. method for supporting the ring and thermometer may be used,
provided it meets the following requirements:
12. Report 13.2.1 The ring must be supported in a substantially hori-
zontal position.
12.1 Report the softening point to the nearest 1.0°C. 13.2.2 When using the apparatus shown in Fig. 1(d): The
12.2 Report the bath liquid used in the test. bottom of the ring must be 25.4 6 0.2 mm (1.0 in.) above the

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 E28 − 18
horizontal plate below it; the bottom surface of the horizontal Center the ball on the surface of the test specimen in the ring.
plate must be 12.7 to 19.05 mm (0.5 to 0.75 in.) above the Suspend an ASTM low-softening-point thermometer in the
bottom of the beaker. bath as prescribed in 13.2.3. Maintain the initial temperature of
13.2.3 Suspend a thermometer so that the bottom of the bulb the water for 15 min. Start stirring, and continue stirring until
is level with the bottom of ring and within 12.7 mm (0.5 in.) completion of the determination.
but not touching the ring or the ring holder. 14.2 Heating—Heat the bath so that the temperature of the
13.3 Bath—A heat-resistant glass beaker, at least 85 mm water is raised uniformly at a rate of 5°C (10°F)/min. Protect
(3.34 in.) in diameter and 127 mm (5 in.) in depth from the the bath from drafts, using shields if necessary. Do not average
bottom of the flare, for example, an 800-mL low-form Griffin the rate of rise over the test period. The maximum permissible
beaker. variation for any 1 min period after the first three minutes is
13.4 Temperature Measuring Device—A thermometer hav- 60.5°C (61°F). Reject any test in which the rate of tempera-
ing a range described below and conforming to the require- ture rise does not fall within these limits.
ments prescribed in Specification E1, or an electronic tempera- NOTE 7—Rigid adherence to the prescribed rate of heating is absolutely
ture measuring device, such as a resistance thermometer or essential for reproducibility of results.
thermocouple. The device must exhibit the same temperature 14.3 Softening Point—Record as the softening point the
response as the thermometers specified in Specification E1 and temperature of the thermometer at the instant the material
must be accurately calibrated. touches the lower horizontal plate (Fig. 1(d)). Make no
13.4.1 An ASTM Thermometer, having a range from −38 to correction for the emergent stem of the thermometer.
+50°C (−36 to +120°F), ASTM 5C, 5F, or any temperature NOTE 8—When the ball drops through the ring, it should be completely
measuring device having equivalent precision. surrounded by softening resin and should drop straight down to the lower
13.4.2 An ASTM Low-Softening-Point Thermometer, having horizontal plate.
a range from −2 to 80°C (30 to 180°F), ASTM 15C, 15F, or any 14.4 Thoroughly clean the ring holder, ball, and ring in a
temperature measuring device having equivalent precision. suitable solvent.
13.4.3 An ASTM Medium-Softening Point Thermometer,
having a range from 30 to 200°C (85 to 392°F), ASTM 16C, 15. Calibration
16F, or any temperature measuring device having equivalent 15.1 A calibration check of any temperature controllers used
precision. in the manual ring and ball softening point apparatus must be
13.4.4 An ASTM High-Softening-Point Thermometer, hav- performed on a regular basis since accurate temperature control
ing a range from −2 to 300°C (30 to 580°F), ASTM 7C, 7F, or is required.
any temperature measuring device having equivalent precision.
13.5 Stirer—The heating bath must be stirred at a speed 16. Procedure for Materials Having Softening Points
sufficient to ensure uniform heat distribution without causing Between 80°C (176°F) and 150°C (302°F)
significant sideways displacement of the resin as it softens in 16.1 Use the same procedure as described in Section 14,
the ring. A stirring rate of 500 to 700 r/min is typical. A except fill the bath with glycerin or silicone oil (Note 9) and
mechanical motor-driven stirrer, mounted so that any vibra- use an ASTM medium-softening-point thermometer. The
tions created by its rotation are not conveyed directly to the maximum allowable starting temperature of the bath is the
sample support, or a magnetic stirrer placed under the bath may lower of: (a) 27°C (81°F) below the anticipated softening
be used. point, or (b) 32°C (90°F).
NOTE 9—For materials softening around 80°C (176°F) report the bath
13.6 Heat Source—A heat source capable of maintaining the liquid since a glycerin or silicone oil bath will yield a slightly higher result
proper heating rate, such as a temperature controller with than a water bath.
immersion heating coil, an electric heater or a bunsen burner. NOTE 10—Repeated use of glycerin will increase the moisture content
over time and may affect results. Replace with fresh glycerin if any change
14. Procedure for Materials Having a Softening Point in appearance is noted.
Between 35°C (95°F) and <80°C (176°F)
17. Procedure for Materials Having Softening Points
14.1 Assembly of Apparatus—Fill the bath with distilled or Above 150°C (302°F)
deionized water, conforming to the requirements in 5.1.1, so 17.1 Use the same procedure as described in Section 14,
that the level will be 105 6 3 mm (4.13 6 0.12 in.). If a except fill the bath with silicone oil (Note 4) and use an ASTM
mechanical motor-driven stirrer is used, position the axis of the high-softening-point thermometer.
stirrer shaft near the back wall of the beaker, with the blades
clearing the wall and with the bottom of the blades approxi- 18. Procedure for Materials Having Softening Points
mately 19.0 mm (0.75 in.) above the top of the ring. If the Below 35°C (95°F)
ball-centering guide is not used, make a slight indentation in
the center of the sample by pressing the ball or a rounded rod, 18.1 Apparatus:
slightly heated for hard materials, into the material at this point. 18.1.1 Freezer or Isopropyl Alcohol Dry-Ice Bath.
Suspend the ring containing the sample in the water in the 18.2 Procedure:
manner described in 13.2.2 or 25.4 6 0.2 mm (1 in.) above the 18.2.1 Cool the bath, described in 5.1.4.1, to −25°C (−13°F)
bottom of the beaker when using the apparatus in Fig. 2(e). in a freezer or isopropyl alcohol dry-ice bath.

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 E28 − 18

FIG. 2 Assembly of Apparatus Showing Stirrer and Single Shouldered Ring

18.2.2 Use the same procedure as in Section 14 except for 20.1.2 Precision:
the bath liquid. Immediately begin heating as directed once the 20.1.2.1 For a material having a 70°C ring and ball soften-
test specimen in the ring has been placed in the bath. ing point run in a water bath:
(1) Repeatability Limit, 95 % (within laboratory) = 0.9°
19. Report (2) Reproducibility Limit, 95 % (between laboratories) = 2.4°
19.1 Report the softening point to the nearest 1.0°C. 20.1.2.2 For a material having a 100 to 135°C ring and ball
19.2 Report the bath liquid used in the test. softening point run in a glycerin or silicone oil bath:
(1) Repeatability Limit, 95 % (within laboratory) = 1.3°
20. Precision and Bias4 (2) Reproducibility Limit, 95 % (between laboratories) = 3.9°

20.1 Automatic Method Precision—An interlaboratory 20.1.2.3 The above terms (repeatability limit and reproduc-
study of the ring and ball softening point of three hydrocarbon ibility limit) are used as specified in Practice E177. The
resins was run in 1998 by 21 laboratories. The design of the respective standard deviations among test results, related to the
experiment, similar to that of Practice E691, and a within- above numbers by the factor 2.8, are:
between analysis of the data are given in ASTM Research 20.1.2.4 For a material having a 70°C ring and ball soften-
Report No. RR:D01-1113. ing point run in a water bath:
20.1.1 Test Result—The precision information given below (1) Repeatability Standard Deviation = 0.3°
(2) Reproducibility Standard Deviation = 0.9°
for ring and ball softening point of a hydrocarbon resin at the
70°C level in a water bath, and for hydrocarbon resins at the 20.1.2.5 For a material having a 100 to 135°C ring and ball
100 to 135°C level in a glycerin or silicone oil bath, softening point run in a glycerin or silicone oil bath:
respectively, is for the comparison of two test results. (1) Repeatability Standard Deviation = 0.5°
(2) Reproducibility Standard Deviation = 1.4°

4
Supporting data have been filed at ASTM International Headquarters and may
20.2 Manual Method Precision—An interlaboratory study
be obtained by requesting Research Report RR:D01-1113. Contact ASTM Customer of the ring and ball-softening point of rosin and three resins
Service at service@astm.org. was run in 1995 by 9 laboratories. The design of the

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 E28 − 18
experiment, similar to that of Practice E691, and a within- respective standard deviations among test results, related to the
between analysis of the data are given in ASTM Research above numbers by the factor 2.8, are:
Report No. D01-1113. 20.2.2.4 For a material having a 75°C ring and ball soften-
20.2.1 Test Result—The precision information given below ing point run in a water bath:
for ring and ball softening point of rosin at the 75°C level in a
(1) Repeatability Standard Deviation = 0.3°
water bath, and for resins at the 100 to 140°C level in a (2) Reproducibility Standard Deviation = 2.1°
glycerin or silicone oil bath, respectively, is for the comparison
of two test results. 20.2.2.5 For a material having a 100 to 140°C ring and ball
20.2.2 Precision: softening point run in a glycerin or silicone oil bath:
20.2.2.1 For a material having a 75°C ring and ball soften- (1) Repeatability Standard Deviation = 0.4°
(2) Reproducibility Standard Deviation = 2.2°
ing point run in a water bath:
(1) Repeatability Limit, 95 % (within laboratory) = 0.8° 20.3 Bias—Since there is no accepted reference material,
(2) Reproducibility Limit, 95 % (between laboratories) = 5.9° method or laboratory suitable for determining the bias for the
20.2.2.2 For a material having a 100 to 140°C ring and ball procedure in this test method for measuring the ring and ball
softening point run in a glycerin or silicone oil bath: softening point, no statement on bias is being made.
(1) Repeatability Limit, 95 % (within laboratory) = 1.2°
(2) Reproducibility Limit, 95 % (between laboratories) = 6.1° 21. Keywords
20.2.2.3 The above terms (repeatability limit and reproduc- 21.1 polyterpene resins; ring and ball; rosin; softening point
ibility limit) are used as specified in Practice E177. The

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