ASTM D6493-05(2010)
(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
SIGNIFICANCE AND USE
For hydrocarbon 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 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 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:D6493–05(Reapproved2010)
Standard Test Methods for
Softening Point of Hydrocarbon 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* ISO 4625 Binders for paints and varnishes—Determination
of softening point–Ring-and-ball method
1.1 These test methods are intended for determining the
softening point of hydrocarbon resins and similar materials by
3. Summary of Test Method
means of an automated ring-and-ball apparatus. Portions are
3.1 These test methods are for the determination of a
similar in technical content to the automated-apparatus ver-
hydrocarbon resin’s softening point—the temperature at which
sions of Test Methods D36, E28, and ISO 4625.
a disk of the resin held within a horizontal ring is forced
1.1.1 The ring-and-ball softening point of a hydrocarbon
downwardadistanceof25.4mm(1.00in.)undertheweightof
resin may also be determined with lower precision using the
a standard steel ball, as the specimen is heated at 5°C/min. in
manual ring-and-ball softening point procedure in Test Meth-
a specified liquid bath.
ods 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, softening does not take place at
only.
adefinitetemperature.Asthetemperaturerises,thesematerials
1.3 This standard method does not purport to address all of
gradually change from brittle solids or very viscous liquids to
the safety concerns, if any, associated with its use. It is the
less viscous liquids. For this reason, determination of the
responsibility of the user of this standard to establish appro-
softening point must be made by a fixed, arbitrary, and closely
priate safety and health practices and determine the applica-
defined method if the results obtained are to be comparable.
bility of regulatory limitations prior to use.
5. Sample Preparation
2. Referenced Documents
2 5.1 Preparation of Sample by the Pour Method: This
2.1 ASTM Standards:
procedure is suitable for resins that can be heated and poured
D36 Test Method for Softening Point of Bitumen (Ring-
without adverse effect on the softening point.
and-Ball Apparatus)
5.1.1 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 broken
E28 Test Methods for Softening Point of Resins Derived
lumps. Avoid inclusion of finely divided material or dust.
from Naval Stores by Ring-and-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
Determine the Precision of a Test Method
slowly, taking care to avoid incorporating air bubbles in the
2.2 ISO Standard:
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
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct
min.
responsibility of Subcommittee D01.34 on Pine Chemicals and Hydrocarbon
5.1.3 Formaterialsthattendtocrackorshrinkintheringon
Resins.
cooling, immediately before filling the ring, preheat the ring to
Current edition approved July 15, 2010. Published September 2010. Originally
approximately the temperature at which the material is to be
approved in 1999. Last previous edition approved in 2005 as D6493 – 05. DOI:
10.1520/D6493-05R10.
poured. The ring, while being filled, should rest bottom down
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.
*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.
D6493–05 (2010)
(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 temperature-measuring device (in accordance with
cannot be heated and poured without adverse effects on the
Specification E1), a heating unit, a heating-rate controller, and
softening point. See Appendix X1.1, Alternate Sample Prepa-
a digital temperature display.
ration Procedures.
6.2 Ring—A brass, shouldered ring conforming to the
5.3 Preparation of Samples Having a Low Softening Point
dimensions shown in Fig. 1(a).
(up to 35°C (95°F)):
6.3 Ball—A steel ball, 9.53 6 0.1 mm ( ⁄8 in.) in diameter,
5.3.1 Place a ring on a piece of aluminum foil. Pour the
weighing between 3.45 and 3.55 g.
material to be tested into the ring, then place the foil and the
6.4 Ball-Centering Guide (optional), having the dimensions
filled ring on dry ice or in a freezer to cool. The material in the
ring must be free of bubbles. given in Fig. 1(c).
FIG. 1 Shouldered Ring, Ring Holder, Ball-Centering Guide, and Assembly of Apparatus
D6493–05 (2010)
6.5 Beaker, 600 mL, borosilicate glass, to hold the bath ments in 7.1.1. Ensure that the beaker is properly positioned on
liquid. ensure that the dimensions will properly fit the heating the heater in the test unit. Place the prepared sample rings in
unit. the test assembly. Place a ball-centering guide and ball on top
6.6 Stirrer—Either a magnetic stirring motor and a mag- of each sample ring. Place the test assembly in the beaker.
netic stir bar, or a direct-driven agitator with a stirring motor. Place the temperature-measuring device in the opening in the
The dimensions of a stir bar must be such that the bar spins cover of the test assembly. Verify that the control unit is set for
freely under the test assembly. The bath must be stirred at a the correct bath liquid.
speed sufficient to ensure uniform temperature distribution 9.2 Heat the bath so that the temperature of the water is
without causing significant sideways displacement of the resin raised uniformly at a rate of 5°C (10°F)/min. Protect the bath
as it sags below the ring. from drafts, using shields if necessary. Reject any test in which
the rate of temperature rise does not fall within these limits.
7. Reagents and Materials
The test is complete when the light beam has been interrupted
7.1 Bath Liquids: by the falling ball and material.
7.1.1 Distilled or Deionized Water, Freshly Boiled—For
NOTE 3—Rigid adherence to the prescribed rate of heating is absolutely
softening points between 35°C (95°F) and 80°C (176°F).
essential for reproducibility of results.
7.1.1.1 Usedistilledordeionizedwaterthathasbeencooled
9.3 Record as the softening point the temperature displayed
to at least 27°C (81°F) below the anticipated softening point,
on the unit after the light beam has been interrupted by the
but in no case lower than 5°C (41°F).
falling ball and material.
7.1.2 USP Glycerin—For softening points between 80°C
9.4 Start the cooling process in the instrument. Remove the
(176°F) and 150°C (302°F). Repeated use of glycerin (over
temperaturemeasuringdevicefromthetestinsert,thenremove
about four heating cycles) may affect results. Open storage of
the test insert from the beakers. Thoroughly clean the test
glycerin can increase the moisture content, which may affect
insert, ball, and ring in a suitable solvent.
results. Replace with fresh glycerin if any change in appear-
ance or viscosity is noted. Use fresh glycerin for referee work.
10. Procedure for Materials Having Softening Points
Warning—Glycerin must not be used for softening points
Between 80°C (176°F) and 150°C (302°F)
greater than 150°C (302°F) due to the 160°C (320°F) flash
10.1 Use the same procedur
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D6493–05 Designation: D6493 – 05 (Reapproved 2010)
Standard Test Methods for
Softening Point of Hydrocarbon 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*
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. 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 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 Naval Stores 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 a hydrocarbon resin’s 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, 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.
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
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 July 1, 2005.15, 2010. Published August 2005.September 2010. Originally approved in 1999. Last previous edition approved in 19992005 as
D6493–99.D6493 – 05. DOI: 10.1520/D6493-05R10.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. ForAnnualBookofASTMStandards
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 – 05 (2010)
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.
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 temperature-measuring device (in accordance with Specification
E1), a heating unit, a heating-rate controller, and a digital temperature display.
FIG. 1 Shouldered Ring, Ring Holder, Ball-Centering Guide, and Assembly of Apparatus
D6493 – 05 (2010)
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 USPGlycerin—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) —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 and 35°C, a 50/50 (v/v) mixture of glycerin and water may be used.
8. Calibration
8.1 The calibration of any automated ring and ball softening point apparatus must be performed on a regular basis, since
accurate temperature control is required. Follow the manufacturer’s instructions for calibration of the instrument.
9. Procedure for Materials Having a Softening Point Betwee
...
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