ASTM D6090-23

Standard Test Method for Softening Point Resins (Mettler Cup and Ball Method)

SIGNIFICANCE AND USE
4.1 In general, with materials of these types, softening point does not take place at a definite temperature. As the temperature rises, these materials gradually change from brittle or exceedingly thick and slow-flowing materials to softer and less viscous liquids. For this reason, the 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 This test method covers the determination of softening point of resins using a Mettler cup and ball apparatus, and may, under user-defined conditions, give results comparable to those obtained by 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: 31-Jan-2023
• ICS: 87.060.20 - Binders
• 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 E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• 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 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 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 E177-06 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-04e1 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-04 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E28-99(2004) - Standard Test Methods for Softening Point of Resins Derived from Naval Stores by Ring-and-Ball Apparatus
• Effective Date: 01-Jun-2004

Overview

ASTM D6090-23 – Standard Test Method for Softening Point Resins (Mettler Cup and Ball Method) is an internationally recognized method for determining the softening point of resins using the Mettler cup and ball apparatus. This test is particularly relevant for resins that do not have a distinct softening temperature, but instead transition gradually from a brittle or highly viscous state to a softer, less viscous liquid as temperature increases. The standard provides a precise and repeatable method to determine the softening point, ensuring consistency and comparability of results across different laboratories and applications.

Key Topics

• Significance of Softening Point Testing

  • The softening point of resins is a critical quality parameter for various industrial processes.
  • As resins do not soften at a fixed temperature, a standard method is necessary for reliable measurements.

• Mettler Cup and Ball Apparatus

  • Utilizes a controlled digital temperature system and precision components to heat samples at a linear rate.
  • The softening point is indicated when the sample flows a set distance upon heating.

• Calibration and Precision

  • Calibration against primary standards (such as benzoic acid) is required to ensure the accuracy of results.
  • Secondary standard materials can be used to match the dropping point of specific resin samples.

• Repeatability and Reproducibility

  • The standard details repeatability limits (within-laboratory) and reproducibility limits (between laboratories).
  • Ensures that results are consistent for quality control and product development.

• Safety and Compliance

  • Users must establish appropriate safety, health, and environmental practices as not all risks are addressed in the standard.

Applications

ASTM D6090-23 is widely used in numerous industries where understanding the thermal behavior of resins is essential:

• Paints and Coatings

  • Essential for determining application and curing conditions for resins used in paints and protective coatings.

• Adhesives and Sealants

  • Assists in formulating products that must function under specific temperature conditions.

• Plastics and Polymers

  • Provides critical quality control data for manufacturing and processing of resin-based materials.

• Quality Assurance and Product Development

  • Used in routine quality assurance testing and in research and development to benchmark product performance.

• Comparison between Methods

  • May provide results comparable to those obtained by ASTM E28 (Ring-and-Ball Softening Point Method) under similar conditions, offering flexibility for users familiar with different standardized methods.

Related Standards

For comprehensive resin testing, users of ASTM D6090-23 should also reference the following key standards:

• ASTM E28 – Test Methods for Softening Point of Resins Derived from Pine Chemicals and Hydrocarbons by Ring-and-Ball Apparatus
  • Provides alternative methodologies for softening point determination.
• ASTM E177 – Practice for Use of the Terms Precision and Bias in ASTM Test Methods
  • Defines the statistical terms and concepts used to report test results.
• ASTM E691 – Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
  • Details protocols for validating test methods through multi-laboratory comparisons.

Practical Value

Adopting ASTM D6090-23 ensures that the softening point of resins is measured in a reproducible, transparent, and internationally recognized manner. This enhances quality control, supports regulatory compliance, and fosters confidence in product performance for end users. The method’s standardization also facilitates global trade by allowing manufacturers and customers to reference a common testing protocol for resin softening point specification.

Keywords: ASTM D6090-23, softening point, Mettler cup and ball method, resin testing, quality control, industrial standards, thermal analysis, paint and coatings, adhesives, polymers.

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: D6090 − 23
Standard Test Method for
Softening Point Resins (Mettler Cup and Ball Method)
This standard is issued under the fixed designation D6090; 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 cup with a 6.35 mm hole in the bottom and with a stainless
steel ball, 8.7 mm in diameter, centered on top of the sample in
1.1 This test method covers the determination of softening
the cup, flows downward a distance of 19 mm to interrupt a
point of resins using a Mettler cup and ball apparatus, and may,
light beam, as the sample is heated at a linear rate in air.
under user-defined conditions, give results comparable to those
obtained by Test Methods E28.
4. Significance and Use
1.2 The values stated in SI units are to be regarded as the
4.1 In general, with materials of these types, softening point
standard. The values given in parentheses are for information
does not take place at a definite temperature. As the tempera-
only.
ture rises, these materials gradually change from brittle or
1.3 This standard does not purport to address all of the
exceedingly thick and slow-flowing materials to softer and less
safety concerns, if any, associated with its use. It is the
viscous liquids. For this reason, the 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, health, and environmental practices and deter-
defined method if the results obtained are to be comparable.
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
5. Apparatus
dance with internationally recognized principles on standard-
5.1 Softening Point Apparatus —This commercially avail-
ization established in the Decision on Principles for the
able instrument consists of a control unit with a digital
Development of International Standards, Guides and Recom-
temperature indicator; matched measuring cell; cartridge
mendations issued by the World Trade Organization Technical
assembly, consisting of a sample cup and upper portion; and
Barriers to Trade (TBT) Committee.
accessories. The control unit automatically regulates the heat-
ing rate of the measuring cell. The softening point is indicated
2. Referenced Documents
on the readout, and the heating program stopped, when the
2.1 ASTM Standards:
sample flow triggers a photocell detector.
E28 Test Methods for Softening Point of Resins Derived
5.2 Central Processor—This unit shall provide a
from Pine Chemicals and Hydrocarbons, by Ring-and-
continuous, linear temperature increase from 25 °C to 375 °C.
Ball Apparatus
E177 Practice for Use of the Terms Precision and Bias in
5.3 Measuring Cell—This unit shall be capable of heating a
ASTM Test Methods
sample cup assembly, as described in 5.4, at a linear rate with
E691 Practice for Conducting an Interlaboratory Study to
an accuracy of 60.2 °C ⁄min. It shall include a sensing system
Determine the Precision of a Test Method
capable of detecting the softening point with a precision of
0.1 °C.
3. Summary of Test Method
5.4 Sample Cup Assembly—A cup of chromium-plated brass
3.1 In this test method, the softening point is defined as the
and an upper portion, conforming to the dimensions shown in
temperature at which the sample, suspended in a cylindrical
Fig. 1.
5.5 Ball—A stainless steel ball, 8.7 mm ( ⁄32 in.) in
1 diameter, weighing 2.77 g 6 0.02 g.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.34 on Pine Chemicals and Hydrocarbon Resins.
Current edition approved Feb. 1, 2023. Published March 2023. Originally
approved in 1997. Last previous edition approved in 2017 as D6090 – 17. DOI: The sole source of supply of the apparatus FP90/FP83HT, known to the
10.1520/D6090-23. committee at this time is the Mettler-Toledo, Inc., Princeton-Hightstown Rd.,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Hightstown, NJ 08520. If you are aware of alternative suppliers, please provide this
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM information to ASTM International Headquarters. Your comments will receive
Standards volume information, refer to the standard’s Document Summary page on careful consideration at a meeting of the responsible technical committee, which
the ASTM website. you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6090 − 23
apparatus carefully to ensure that no residue remains. Wash the
cartridge parts with a suitable solvent to remove the last traces
of the residue.
6.3.4 Interpretation—If the result is not 123.5 °C 6 0.5 °C,
repeat the test. If the second value remains outside of the
acceptable range, repeat the test using a fresh sample of
benzoic acid. If the results remain outside of the acceptable
range, the instrument requires recalibration or repair. Consult
the manufacturer’s instruction manual.
7. Instrument Check of Apparatus Using a Secondary
Standard
7.1 The primary calibration standard, benzoic acid, might
not have a dropping point similar to the softening point of the
resin being tested. In such cases, it is desirable to calibrate the
instrument using a secondary standard having a dropping point
similar to that of the test sample. Materials suitable for use as
secondary standards are listed, but are not limited to those, in
Table 1. Demonstration of conformance to the dropping point
of benzoic acid should be completed before a secondary
FIG. 1 Sample Cup
standard is read.
7.2 Follow the same procedure as in 6.3.2 and 6.3.3 but start
about 3 °C below the actual dropping point of the secondary
6. Calibration of Apparatus Using a Primary Standard
standard.
6.1 This step, required only occasionally, is designed to
8. Preparation of Sample
establish that the temperature indicated by the instrument is in
agreement with a known standard. A special cup with a bottom
8.1 Fold the tab on an oil-free disposable aluminum weigh-
orifice of 2.8 mm is used instead of the one specified for testing
ing dish to a horizontal position and pinch a pour spout into the
the resin.
dish directly opposite the tab. Weigh 5 g to 10 g of resin into
the dish.
NOTE 1—The stainless steel ball is not used during calibration.
8.2 Place the dish and sample on a preheated hot plate and
6.2 Reagent—Use either analytical reagent or primary stan-
cover with a 600 mL or larger beaker. Heat the sample until it
dard grade benzoic acid for the calibration. As this material is
is almost melted.
hygroscopic, it must be stored in a tightly sealed container, and
replaced with fresh material from a newly opened supply if
8.3 Remove the beaker from the hot plate, grasp the tab with
hydration or other contamination is suspected.
forceps or needle-nose pliers, and stir the sample with a
probe-type thermometer until it is completely melted and
6.3 Procedure:
homogeneous. Avoid entraining air into the sample melt. The
6.3.1 Filling the Sample Cup—Place the cup on a clean, flat
temperature of the sample should be no more than 60 °C above
surface and fill it with benzoic acid crystals. Hand press the
the expected softening point. Remove the thermometer and
material into the cup with a 9.2 mm rod of dowel stock or
equivalent. Refill and repeat the pressing step until the
...

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: D6090 − 17 D6090 − 23
Standard Test Method for
Softening Point Resins (Mettler Cup and Ball Method)
This standard is issued under the fixed designation D6090; 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 This test method covers the determination of softening point of resins using a Mettler cup and ball apparatus, and may, under
user-defined conditions, give results comparable to those obtained by 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.
2. Referenced Documents
2.1 ASTM Standards:
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
3. Summary of Test Method
3.1 In this test method, the softening point is defined as the temperature at which the sample, suspended in a cylindrical cup with
a 6.35-mm6.35 mm hole in the bottom and with a stainless steel ball, 88.7 mm in diameter, centered on top of the sample in the
cup, flows downward a distance of 19 mm to interrupt a light beam, as the sample is heated at a linear rate in air.
4. Significance and Use
4.1 In general, with materials of these types, softening point does not take place at a definite temperature. As the temperature rises,
these materials gradually change from brittle or exceedingly thick and slow-flowing materials to softer and less viscous liquids.
For this reason, the determination of the softening point must be made by a fixed, arbitrary, and closely defined method if the results
obtained are to be comparable.
This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.34 on Pine Chemicals and Hydrocarbon Resins.
Current edition approved Dec. 1, 2017Feb. 1, 2023. Published December 2017March 2023. Originally approved in 1997. Last previous edition approved in 20122017 as
D6090 – 12.D6090 – 17. DOI: 10.1520/D6090-17.10.1520/D6090-23.
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 the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6090 − 23
5. Apparatus
5.1 Softening Point Apparatus —This commercially available instrument consists of a control unit with a digital temperature
indicator; matched measuring cell; cartridge assembly, consisting of a sample cup and upper portion; and accessories. The control
unit automatically regulates the heating rate of the measuring cell. The softening point is indicated on the readout, and the heating
program stopped, when the sample flow triggers a photocell detector.
5.2 Central Processor—This unit shall provide a continuous, linear temperature increase from 25 to 375°C.25 °C to 375 °C.
5.3 Measuring Cell—This unit shall be capable of heating a sample cup assembly, as described in 5.4, at a linear rate with an
accuracy of 60.2°C/min.60.2 °C ⁄min. It shall include a sensing system capable of detecting the softening point with a precision
of 0.1°C.0.1 °C.
5.4 Sample Cup Assembly—A cup of chromium-plated brass and an upper portion, conforming to the dimensions shown in Fig.
1.
5.5 Ball—A stainless steel ball, 8.7 mm ( ⁄32 in.) in diameter, weighing 2.772.77 g 6 0.02 g.
6. Calibration of Apparatus Using a Primary Standard
6.1 This step, required only occasionally, is designed to establish that the temperature indicated by the instrument is in agreement
with a known standard. A special cup with a bottom orifice of 2.8 mm is used instead of the one specified for testing the resin.
NOTE 1—The stainless steel ball is not used during calibration.
6.2 Reagent—Use either analytical reagent or primary standard grade benzoic acid for the calibration. As this material is
hygroscopic, it must be stored in a tightly sealed container, and replaced with fresh material from a newly opened supply if
hydration or other contamination is suspected.
6.3 Procedure:
FIG. 1 Sample Cup
The sole source of supply of the apparatus FP90/FP83HT, known to the committee at this time is the Mettler-Toledo, Inc., Princeton-Hightstown Rd., Hightstown, NJ
08520. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at
a meeting of the responsible technical committee, which you may attend.
D6090 − 23
6.3.1 Filling the Sample Cup—Place the cup on a clean, flat surface and fill it with benzoic acid crystals. Hand press the material
into the cup with a 9.2-mm9.2 mm rod of dowel stock or equivalent. Refill and repeat the pressing step until the cup is filled with
benzoic acid. Remove any crystals from the exterior of the cup.
6.3.2 Heating—Preheat the measuring cell to 121°C,121 °C, and maintain it at that temperature. Place the cartridge assembly
containing the benzoic acid in position in the measuring cell, taking care that the slits for the light beam are properly positioned.
With the instrument set in the dropping point mode, start the required method, which includes a waiting period of 30 s to allow
temperature equilibration between the measuring cell and sample followed by an automatic temperature ramp of 0.2°C/
min.0.2 °C ⁄min. The temperature will rise steadily at the correct rate until the drop point is reached, and then remain steady on
the readout.
6.3.3 Cleaning—Immediately remove the cartridge assembly. Check to determine that the sample has passed through the light
beam and no pre-triggering has occurred. If a malfunction is suspected, the entire procedure must be repeated. Inspect the apparatus
carefully to ensure that no residue remains. Wash the cartridge parts with a suitable solvent to remove the last traces of the residue.
6.3.4 Interpretation—If the result is not 123.5 6 0.5°C,123.5 °C 6 0.5 °C, repeat the test. If the second value remains outside of
the acceptable range, repeat the test using a fresh sample of benzoic acid. If the results remain outside of the acceptable range, the
instrument requires recalibration or repair. Consult the manufacturer’s instruction manual.
7. Instrument Check of Apparatus Using a Secondary Standard
7.1 The primary calibration standard, benzoic acid, might not have a dropping point similar to the softening point of the resin being
tested. In such cases, it is desirable to calibrate the instrument using a secondary standard having a dropping point similar to that
of the test sample. Materials suitable fo
...