ASTM D6493-11(2022)

Standard Test Methods for Softening Point of Hydrocarbon Resins and Rosin Based Resins by Automated Ring-and-Ball Apparatus

SIGNIFICANCE AND USE
4.1 For hydrocarbon resins and rosin based resins, softening does not take place at a definite temperature. As the temperature rises, these materials gradually change from brittle solids or very viscous liquids to less viscous liquids. For this reason, 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 These test methods are intended for determining the softening point of hydrocarbon resins, rosin based resins and similar materials by means of an automated ring-and-ball apparatus. Portions are similar in technical content to the automated-apparatus versions of Test Methods D36, E28, and ISO 4625.  
1.1.1 The ring-and-ball softening point of a hydrocarbon resin and rosin based resins may also be determined with lower precision using the manual ring-and-ball softening point procedure in Test Methods E28.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

General Information

• Status: Published
• Publication Date: 30-Nov-2022
• ICS: 83.080.20 - Thermoplastic materials
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.34 - Pine Chemicals and Hydrocarbon Resins

Relations

• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM E177-13 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2013
• Refers: ASTM E1-13 - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-May-2013
• Refers: ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• Refers: ASTM E691-11 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2011
• Refers: ASTM E177-10 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2010
• Refers: ASTM E28-99(2009) - Standard Test Methods for Softening Point of Resins Derived from Naval Stores by Ring-and-Ball Apparatus
• Effective Date: 01-Jun-2009
• Refers: ASTM E691-08 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Oct-2008
• Refers: ASTM E177-08 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2008
• Refers: ASTM E1-07 - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-Nov-2007
• Refers: ASTM D36-06 - Standard Test Method for Softening Point of Bitumen (Ring-and-Ball Apparatus)
• Effective Date: 01-Dec-2006
• Refers: ASTM E177-06b - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 15-Nov-2006
• Refers: ASTM E177-06a - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2006
• Refers: ASTM E691-05 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2005
• Refers: ASTM E1-05 - Standard Specification for ASTM Liquid-in-Glass Thermometers
• Effective Date: 01-Nov-2005

Overview

ASTM D6493-11(2022) specifies standard test methods for determining the softening point of hydrocarbon resins and rosin based resins using an automated ring-and-ball apparatus. These procedures ensure consistent, comparable results for materials that gradually transition from brittle solids or viscous liquids to less viscous liquids as temperature increases. This standard supports quality control, product specification, and research in industries using hydrocarbon and rosin based resins.

Key Topics

• Automated Ring-and-Ball Test Method: The core procedure involves heating a resin sample within a standardized ring, placed in a liquid bath, and using a metal ball to determine the temperature at which the

sample softens and sags below the ring. The test is performed with strict temperature rise rates and specific apparatus requirements to ensure repeatable results.

• Scope of Materials: Applicable to hydrocarbon resins, rosin based resins, and similar substances where softening does not occur at a single, distinct temperature but over a range.

• Sample Preparation: Multiple methods are outlined, including pour and powder methods, to accommodate varying physical forms and thermal sensitivities of the resin materials.

• Test Conditions and Calibration: Details on the use of distilled water, glycerin, silicone oil, or ethylene glycol as bath fluids, depending on the anticipated softening point, and the importance of regular calibration of instruments are emphasized.

• Precision and Reporting: Specifies precision limits, repeatability, and reproducibility for different temperature ranges to enhance inter- and intra-laboratory consistency.

Applications

• Quality Control in Manufacturing: Accurate determination of softening points is critical for production quality assurance in adhesives, coatings, paints, varnishes, and sealants utilizing hydrocarbon or rosin based resins.

• Product Development: Essential for characterizing thermal properties of resins to ensure performance in end-use environments.

• Material Comparison and Specification: Enables suppliers and users of hydrocarbon and rosin based resins to compare batch quality and comply with customer or regulatory specifications.

• Research and Development: Serves as a standardized method for academic and industrial research focused on resin formulation, modification, and performance characterization.

Related Standards

• ASTM D36 - Standard Test Method for Softening Point of Bitumen (Ring-and-Ball Apparatus): Provides a similar ring-and-ball approach for bitumen, aligning procedures for comparable materials.

• ASTM E28 - Test Methods for Softening Point of Resins Derived from Pine Chemicals and Hydrocarbons: Offers a manual test counterpart for certain resins with guidance on scope overlap.

• ISO 4625 - Binders for Paints and Varnishes - Determination of Softening Point (Ring-and-Ball Method): International equivalence, supporting compatibility of test results for global trade and regulatory compliance.

• ASTM E177 and ASTM E691: Outline terms, practices, and statistical approaches for test method precision and interlaboratory studies.

Practical Value

Implementing ASTM D6493-11(2022) enables laboratories and production facilities to achieve reliable, standardized measurements of the softening point of hydrocarbon and rosin based resins. This ensures compatibility, quality assurance, and facilitates international trade and regulatory compliance. By following this test method, organizations support the reproducibility and comparability of key thermal property data across the supply chain.

Keywords: ASTM D6493, softening point test, hydrocarbon resins, rosin based resins, automated ring-and-ball, thermal analysis, quality control, standard test method.

Standards Content (Sample)

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: D6493 − 11 (Reapproved 2022)
Standard Test Methods for
Softening Point of Hydrocarbon Resins and Rosin Based
Resins by Automated Ring-and-Ball Apparatus
This standard is issued under the fixed designation D6493; 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 E28 Test Methods for Softening Point of Resins Derived
from Pine Chemicals and Hydrocarbons, by Ring-and-
1.1 These test methods are intended for determining the
Ball Apparatus
softening point of hydrocarbon resins, rosin based resins and
E177 Practice for Use of the Terms Precision and Bias in
similar materials by means of an automated ring-and-ball
ASTM Test Methods
apparatus. Portions are similar in technical content to the
E691 Practice for Conducting an Interlaboratory Study to
automated-apparatus versions of Test Methods D36, E28, and
Determine the Precision of a Test Method
ISO 4625.
2.2 ISO Standard:
1.1.1 The ring-and-ball softening point of a hydrocarbon
ISO 4625 Binders for paints and varnishes—Determination
resinandrosinbasedresinsmayalsobedeterminedwithlower
of softening point–Ring-and-ball method
precision using the manual ring-and-ball softening point pro-
cedure in Test Methods E28.
3. Summary of Test Method
1.2 The values stated in SI units are to be regarded as the
3.1 These test methods are for the determination of the
standard. The values given in parentheses are for information
softening point—the temperature at which a disk of the resin
only.
held within a horizontal ring is forced downward a distance of
1.3 This standard does not purport to address all of the
25.4 mm (1.00 in.) under the weight of a standard steel ball, as
safety concerns, if any, associated with its use. It is the
the specimen is heated at 5 °C⁄min. in a specified liquid bath.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4. Significance and Use
mine the applicability of regulatory limitations prior to use.
4.1 For hydrocarbon resins and rosin based resins, softening
1.4 This international standard was developed in accor-
does not take place at a definite temperature. As the tempera-
dance with internationally recognized principles on standard-
ture rises, these materials gradually change from brittle solids
ization established in the Decision on Principles for the
or very viscous liquids to less viscous liquids. For this reason,
Development of International Standards, Guides and Recom-
determination of the softening point must be made by a fixed,
mendations issued by the World Trade Organization Technical
arbitrary, and closely defined method if the results obtained are
Barriers to Trade (TBT) Committee.
to be comparable.
2. Referenced Documents
5. Sample Preparation
2.1 ASTM Standards:
5.1 Preparation of Sample by the Pour Method: This
D36 Test Method for Softening Point of Bitumen (Ring-and-
procedure is suitable for resins that can be heated and poured
Ball Apparatus)
without adverse effect on the softening point.
E1 Specification for ASTM Liquid-in-Glass Thermometers
5.1.1 Select a sample representative of the material to be
tested.The sample should consist of flakes, pastilles, or broken
lumps. Avoid inclusion of finely divided material or dust.
These test methods are under the jurisdiction of ASTM Committee D01 on
5.1.2 Select a quantity of resin having a volume at least
Paint and Related Coatings, Materials, and Applications and are the direct
twice that necessary to fill the desired number of rings, and
responsibility of Subcommittee D01.34 on Pine Chemicals and Hydrocarbon
Resins.
melt it in a clean container, using an oven, hot plate, sand bath
Current edition approved Dec. 1, 2022. Published December 2022. Originally
or oil bath to prevent local overheating. If necessary, stir
approved in 1999. Last previous edition approved in 2015 as D6493 – 11 (2015).
slowly, taking care to avoid incorporating air bubbles in the
DOI: 10.1520/D6493-11R22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6493 − 11 (2022)
sample. Melt the sample completely, but do not heat it above a 5.3 Preparation of Samples Having a Low Softening Point
temperature necessary to pour the material readily. The time (up to 35°C (95°F)):
from the beginning of heating to pouring should not exceed
5.3.1 Place a ring on a piece of aluminum foil. Pour the
15 min.
material to be tested into the ring, then place the foil and the
5.1.3 Formaterialsthattendtocrackorshrinkintheringon
filled ring on dry ice or in a freezer to cool. The material in the
cooling, immediately before filling the ring, preheat the ring to
ring must be free of bubbles.
approximately the temperature at which the material is to be
5.3.2 After cooling, cut and scrape off any excess material
poured. The ring, while being filled, should rest bottom down
using a slightly heated spatula, then slide the ring gently from
(see Fig. 1(a)) on a suitable metal surface. Pour the sample into
thefoil.Placetheringinthesupportingapparatus,andperform
the ring so as to leave an excess on cooling. After cooling a
the softening point determination in accordance with Section
minimum of 30 min, trim off the excess resin from the top and
12.
outsideofthering.Toremoveexcessresinfromthetop,cutthe
excess off cleanly with a heated knife or spatula, or grasp the
6. Apparatus
ring in a pair of tongs and draw the top surface quickly and
firmly over the surface of a heated plate.
6.1 Automated Ring-and-Ball Softening Point Instrument,
NOTE 1—If the determination is repeated, us a clean container and a having a test assembly consisting of: a ring holder, a metal
fresh sample.
plate, and a cover mounted on two support rods (see Fig. 1(b)
and (d)), a built in digital temperature that should be standard-
5.2 Preparation of Sample by the Powder Method: This
ized periodically to ensure that it meets the specifications for
procedure is suitable for high softening-point materials that
cannot be heated and poured without adverse effects on the and gives the same readings as thermometers given in Speci-
fication E1, a digital temperature display, a heating unit and a
softening point. See Appendix X1.1, Alternate Sample Prepa-
ration Procedures. heating-rate controller.
FIG. 1 Shouldered Ring, Ring Holder, Ball-Centering Guide, and Assembly of Apparatus
D6493 − 11 (2022)
6.2 Ring—A brass, shouldered ring conforming to the di- 8. Calibration
mensions shown in Fig. 1(a).
8.1 The calibration of any automated ring and ball softening
point apparatus must be performed on a regular basis, since
6.3 Ball—A steel ball, 9.53 mm 6 0.1 mm ( ⁄8 in.) in
accurate temperature control is required. Follow the manufac-
diameter, weighing between 3.45 g and 3.55 g.
turer’s instructions for calibration of the instrument.
6.4 Ball-Centering Guide (optional), having the dimensions
given in Fig. 1(c). 9. Procedure for Materials Having a Softening Point
Between 35 °C (95 °F) and <80 °C (176 °F)
6.5 Beaker, 600 mL, borosilicate glass, to hold the bath
9.1 Add a stir bar or stirrer to the 600 mL beaker. Add
liquid. ensure that the dimensions will properly fit the heating
approximately 500 mL of water, conforming to the require-
unit.
ments in 7.1.1. Ensure that the beaker is properly positioned on
6.6 Stirrer—Eitheramagneticstirringmotorandamagnetic
the heater in the test unit. Place the prepared sample rings in
stir bar, or a direct-driven agitator with a stirring motor. The
the test assembly. Place a ball-centering guide and ball on top
dimensions of a stir bar must be such that the bar spins freely
of each sample ring. Place the test assembly in the beaker.
under the test assembly. The bath must be stirred at a speed
Place the temperature-measuring device in the opening in the
sufficient to ensure uniform temperature distribution without
cover of the test assembly. Verify that the control unit is set for
causing significant sideways displacement of the resin as it
the correct bath liquid.
sags below the ring.
9.2 Heat the bath so that the temperature of the water is
raised uniformly at a rate of 5 °C (10 °F)⁄min. Protect the bath
7. Reagents and Materials
from drafts, using shields if necessary. Reject any test in which
7.1 Bath Liquids:
the rate of temperature rise does not fall within these limits.
7.1.1 Distilled or Deionized Water, Freshly Boiled—For The test is complete when the light beam has been interrupted
softening points between 3
...