ASTM D6493-11(2015)
(Test Method)Standard Test Methods for Softening Point of Hydrocarbon Resins and Rosin Based Resins by Automated Ring-and-Ball Apparatus
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 method 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 − 11 (Reapproved 2015)
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 Determine the Precision of a Test Method
2.2 ISO Standard:
1.1 These test methods are intended for determining the
ISO 4625 Binders for paints and varnishes—Determination
softening point of hydrocarbon resins, rosin based resins and
of softening point–Ring-and-ball method
similar materials by means of an automated ring-and-ball
apparatus. Portions are similar in technical content to the
3. Summary of Test Method
automated-apparatus versions of Test Methods D36, E28, and
3.1 These test methods are for the determination of the
ISO 4625.
softening point—the temperature at which a disk of the resin
1.1.1 The ring-and-ball softening point of a hydrocarbon
held within a horizontal ring is forced downward a distance of
resinandrosinbasedresinsmayalsobedeterminedwithlower
25.4 mm (1.00 in.) under the weight of a standard steel ball, as
precision using the manual ring-and-ball softening point pro-
the specimen is heated at 5°C/min. in a specified liquid bath.
cedure in Test Methods E28.
1.2 The values stated in SI units are to be regarded as the
4. Significance and Use
standard. The values given in parentheses are for information
4.1 For hydrocarbon resins and rosin based resins, softening
only.
does not take place at a definite temperature. As the tempera-
1.3 This standard method does not purport to address all of
ture rises, these materials gradually change from brittle solids
the safety concerns, if any, associated with its use. It is the
or very viscous liquids to less viscous liquids. For this reason,
responsibility of the user of this standard to establish appro-
determination of the softening point must be made by a fixed,
priate safety and health practices and determine the applica-
arbitrary, and closely defined method if the results obtained are
bility of regulatory limitations prior to use.
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
E28 Test Methods for Softening Point of Resins Derived
tested.The sample should consist of flakes, pastilles, or broken
from Pine Chemicals and Hydrocarbons, by Ring-and-
lumps. Avoid inclusion of finely divided material or dust.
Ball Apparatus
5.1.2 Select a quantity of resin having a volume at least
E177 Practice for Use of the Terms Precision and Bias in
twice that necessary to fill the desired number of rings, and
ASTM Test Methods
melt it in a clean container, using an oven, hot plate, sand bath
E691 Practice for Conducting an Interlaboratory Study to
or oil bath to prevent local overheating. If necessary, stir
slowly, taking care to avoid incorporating air bubbles in the
sample. Melt the sample completely, but do not heat it above a
These test methods are under the jurisdiction of ASTM Committee D01 on
temperature necessary to pour the material readily. The time
Paint and Related Coatings, Materials, and Applications and are the direct
from the beginning of heating to pouring should not exceed 15
responsibility of Subcommittee D01.34 on Pine Chemicals and Hydrocarbon
Resins.
min.
Current edition approved Dec. 1, 2015. Published December 2015. Originally
5.1.3 Formaterialsthattendtocrackorshrinkintheringon
approved in 1999. Last previous edition approved in 2011 as D6493 – 11. DOI:
cooling, immediately before filling the ring, preheat the ring to
10.1520/D6493-11R15.
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
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 (2015)
approximately the temperature at which the material is to be filled ring on dry ice or in a freezer to cool. The material in the
poured. The ring, while being filled, should rest bottom down ring must be free of bubbles.
(see Fig. 1(a)) on a suitable metal surface. Pour the sample into
5.3.2 After cooling, cut and scrape off any excess material
the ring so as to leave an excess on cooling. After cooling a
using a slightly heated spatula, then slide the ring gently from
minimum of 30 min., trim off the excess resin from the top and
thefoil.Placetheringinthesupportingapparatus,andperform
outsideofthering.Toremoveexcessresinfromthetop,cutthe
the softening point determination in accordance with Section
excess off cleanly with a heated knife or spatula, or grasp the
12.
ring in a pair of tongs and draw the top surface quickly and
firmly over the surface of a heated plate.
6. Apparatus
NOTE 1—If the determination is repeated, us a clean container and a
6.1 Automated Ring-and-Ball Softening Point Instrument,
fresh sample.
having a test assembly consisting of: a ring holder, a metal
5.2 Preparation of Sample by the Powder Method: This
plate, and a cover mounted on two support rods (see Fig. 1(b)
procedure is suitable for high softening-point materials that
and (d)), a built in digital temperature that should be standard-
cannot be heated and poured without adverse effects on the
ized periodically to ensure that it meets the specifications for
softening point. See Appendix X1.1, Alternate Sample Prepa-
and gives the same readings as thermometers given in Speci-
ration Procedures.
fication E1, a digital temperature display, a heating unit and a
5.3 Preparation of Samples Having a Low Softening Point
heating-rate controller.
(up to 35°C (95°F)):
6.2 Ring—A brass, shouldered ring conforming to the di-
5.3.1 Place a ring on a piece of aluminum foil. Pour the
material to be tested into the ring, then place the foil and the mensions shown in Fig. 1(a).
FIG. 1 Shouldered Ring, Ring Holder, Ball-Centering Guide, and Assembly of Apparatus
D6493 − 11 (2015)
6.3 Ball—A steel ball, 9.53 6 0.1 mm ( ⁄8 in.) in diameter, accurate temperature control is required. Follow the manufac-
weighing between 3.45 and 3.55 g. turer’s instructions for calibration of the instrument.
6.4 Ball-Centering Guide (optional), having the dimensions
9. Procedure for Materials Having a Softening Point
given in Fig. 1(c).
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
7. Reagents and Materials raised uniformly at a rate of 5°C (10°F)/min. Protect the bath
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 35°C (95°F) and 80°C (176°F).
by the falling ball and material.
7.1.1.1 Usedistilledordeionizedwaterthathasbeencooled
to at least 27°C (81°F) below the anticipated softening point,
NOTE 3—Rigid adherence to the prescribed rate of heating is absolutely
but in no case lower than 5°C (41°F). essential for reproducibility of results.
7.1.2 USP Glycerin—For softe
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D6493 − 11 D6493 − 11 (Reapproved 2015)
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*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 method 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.
2. Referenced Documents
2.1 ASTM Standards:
D36 Test Method for Softening Point of Bitumen (Ring-and-Ball Apparatus)
E1 Specification for ASTM Liquid-in-Glass Thermometers
E28 Test Methods for Softening Point of Resins Derived from Pine Chemicals and Hydrocarbons, by Ring-and-Ball Apparatus
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 ISO Standard:
ISO 4625 Binders for paints and varnishes—Determination of softening point–Ring-and-ball method
3. Summary of Test Method
3.1 These test methods are for the determination of the softening point—the temperature at which a disk of the resin held within
a horizontal ring is forced downward a distance of 25.4 mm (1.00 in.) under the weight of a standard steel ball, as the specimen
is heated at 5°C/min. in a specified liquid bath.
4. 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.
5. Sample Preparation
5.1 Preparation of Sample by the Pour Method: This procedure is suitable for resins that can be heated and poured without
adverse effect on the softening point.
These test methods are under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and are the direct responsibility of
Subcommittee D01.34 on Pine Chemicals and Hydrocarbon Resins.
Current edition approved June 1, 2011Dec. 1, 2015. Published June 2011December 2015. Originally approved in 1999. Last previous edition approved in 20102011 as
D6493 – 05 (2010).D6493 – 11. DOI: 10.1520/D6493-11.10.1520/D6493-11R15.
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6493 − 11 (2015)
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.
5.1.2 Select a quantity of resin having a volume at least twice that necessary to fill the desired number of rings, and melt it in
a clean container, using an oven, hot plate, sand bath or oil bath to prevent local overheating. If necessary, stir slowly, taking care
to avoid incorporating air bubbles in the sample. Melt the sample completely, but do not heat it above a temperature necessary to
pour the material readily. The time from the beginning of heating to pouring should not exceed 15 min.
5.1.3 For materials that tend to crack or shrink in the ring on cooling, immediately before filling the ring, preheat the ring to
approximately the temperature at which the material is to be poured. The ring, while being filled, should rest bottom down (see
Fig. 1(a)) 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 min., trim off the excess resin from the top and outside of the ring. To remove excess resin from the top, cut the excess off
cleanly with a heated knife or spatula, or grasp the ring in a pair of tongs and draw the top surface quickly and firmly over the
surface of a heated plate.
NOTE 1—If the determination is repeated, us a clean container and a fresh sample.
5.2 Preparation of Sample by the Powder Method: This procedure is suitable for high softening-point materials that cannot be
heated and poured without adverse effects on the softening point. See Appendix X1.1, Alternate Sample Preparation Procedures.
5.3 Preparation of Samples Having a Low Softening Point (up to 35°C (95°F)):
5.3.1 Place a ring on a piece of aluminum foil. Pour the material to be tested into the ring, then place the foil and the filled ring
on dry ice or in a freezer to cool. The material in the ring must be free of bubbles.
5.3.2 After cooling, cut and scrape off any excess material using a slightly heated spatula, then slide the ring gently from the
foil. Place the ring in the supporting apparatus, and perform the softening point determination in accordance with Section 12.
FIG. 1 Shouldered Ring, Ring Holder, Ball-Centering Guide, and Assembly of Apparatus
D6493 − 11 (2015)
6. Apparatus
6.1 Automated Ring-and-Ball Softening Point Instrument, having a test assembly consisting of: a ring holder, a metal plate, and
a cover mounted on two support rods (see Fig. 1(b) and (d)), a built in digital temperature that should be standardized periodically
to ensure that it meets the specifications for and gives the same readings as thermometers given in Specification E1, a digital
temperature display, a heating unit and a heating-rate controller.
6.2 Ring—A brass, shouldered ring conforming to the dimensions shown in Fig. 1(a).
6.3 Ball—A steel ball, 9.53 6 0.1 mm ( ⁄8 in.) in diameter, weighing between 3.45 and 3.55 g.
6.4 Ball-Centering Guide (optional), having the dimensions given in Fig. 1(c).
6.5 Beaker, 600 mL, borosilicate glass, to hold the bath liquid. ensure that the dimensions will properly fit the heating unit.
6.6 Stirrer—Either a magnetic stirring motor and a magnetic stir bar, or a direct-driven agitator with a stirring motor. The
dimensions of a stir bar must be such that the bar spins freely under the test assembly. The bath must be stirred at a speed sufficient
to ensure uniform temperature distribution without causing significant sideways displacement of the resin as it sags below the ring.
7. Reagents and Materials
7.1 Bath Liquids:
7.1.1 Distilled or Deionized Water, Freshly Boiled—For softening points between 35°C (95°F) and 80°C (176°F).
7.1.1.1 Use distilled or deionized water that has been cooled to at least 27°C (81°F) below the anticipated softening point, but
in no case lower than 5°C (41°F).
7.1.2 USP Glycerin—For softening points between 80°C (176°F) and 150°C (302°F). Repeated use of glycerin (over about four
heating cycles) may affect results. Open storage of glycerin can increase the moisture content, which may affect results. Replace
with fresh glycerin if any change in appearance or viscosity is noted. Use fresh glycerin for referee work. Warning—Glycerin
must not be used for softening points greater than 150°C (302°F) due to the 160°C (320°F) flash point of glycerin.
7.1.3 Silicone Oil (Polydimethylsiloxane) —(Polydimethylsiloxane)—For softening points above 80°C (176°F). The oil must
have a temperature range of 60 to 200°C+ (140 to 392°F+), remain clear throughout the temperature range, have no apparent effect
or reactivity with the test specimen, remain free of moisture, and maintain a relatively uniform viscosity and stirring rate within
the temperature range.
NOTE 2—Replace with fresh silicone oil if any change in appearance is noted. Do not use silicone oil that contains any gels; gels are an indicator that
degradation has occurred.
7.1.4 Ethylene Glycol—For softening points up to 35°C (95°F).
7.1.4.1 Prepare a fresh 50/50 (volume/volume) mixture of distilled water and ethylene glycol prior to softening point
determination. Alternatively, for softening points between 0°C
...
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