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ASTM D4499-07

(Test Method)

Standard Test Method for Heat Stability of Hot-Melt Adhesives

Standard Test Method for Heat Stability of Hot-Melt Adhesives

SIGNIFICANCE AND USE
Hot-melt adhesives must generally be applied at relatively high temperatures in order that the adhesive viscosity is low enough that it can be readily handled in typical hot-melt equipment. Changes in the adhesive caused by exposure to the severe environment required during hot-melt processing will disrupt the adhesive application process and may affect the quality of the adhesive bond. Changes in adhesive viscosity may affect the quantity of adhesive dispensed by the applicator. Phase separation or changes in viscosity and color may be an indication of changes occurring in the adhesive which could affect the quality of the adhesive joint. A skin formed on the adhesive may eventually clog the applicator nozzle or die.
The data generated in this test procedure are comparative in nature. Results can be useful in observing batch-to-batch variation or relative thermal stability of alternate adhesive formulations. Results can also be useful in selecting application equipment and establishing operating conditions for satisfactory handling of a particular hot-melt adhesive.
Round-robin testing showed that the reproducibility of this test method can depend strongly on the characteristics of the adhesive being tested. Results showed that, for the particular adhesives tested in the round robin, the test method was well suited for testing the heat stability of the adhesives based on an EVA copolymer, a polyolefin, and a polyamide. However, because of poor reproducibility, the test method proved to be unsuitable for assessing the heat stability of the adhesive based on a block copolymer. Precision of this test method is discussed in Section 11.
SCOPE
1.1 This test method covers the evaluation of hot-melt adhesives with respect to the change in properties that occurs while the adhesive is aged in the molten state during hot-melt application. Melt properties monitored are viscosity, color, skin formation, and phase separation.
1.2 The values stated in SI units are to be regarded as the standard.
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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
30-Apr-2007
ICS
83.180 - Adhesives
Technical Committee
D10 - Packaging
Drafting Committee
D10.14 - Tape and Labels
Current Stage
Ref Project

Relations

Replaces
ASTM D4499-95(2000) - Standard Test Method for Heat Stability of Hot-Melt Adhesives
Effective Date
01-May-2007
Referred By
ASTM D907-15(2023) - Standard Terminology of Adhesives
Effective Date
01-May-2007
Referred By
ASTM D6465-99(2016) - Standard Guide for Selecting Aerospace and General Purpose Adhesives and Sealants
Effective Date
01-May-2007

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ASTM D4499-07 - Standard Test Method for Heat Stability of Hot-Melt AdhesivesASTM D4499-07 - Standard Test Method for Heat Stability of Hot-Melt Adhesives
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ASTM D4499-07 - Standard Test Method for Heat Stability of Hot-Melt Adhesives
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D4499 − 07
StandardTest Method for
1
Heat Stability of Hot-Melt Adhesives
This standard is issued under the fixed designation D4499; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3.2.2 melt viscosity, n—measure of the ratio of shear stress
to shear rate when the hot-melt is in its molten state.
1.1 This test method covers the evaluation of hot-melt
adhesives with respect to the change in properties that occurs 3.2.3 phase separation, n—formation of a second liquid
while the adhesive is aged in the molten state during hot-melt portion from a previously homogenous liquid over time.
application.Meltpropertiesmonitoredareviscosity,color,skin
3.2.4 skin formation, n—appearance of a relatively loose
formation, and phase separation.
layer at the surface of a polymeric material.
1.2 The values stated in SI units are to be regarded as the
standard. 4. Summary of Test Method
1.3 This standard does not purport to address all of the
4.1 Samples of hot-melt adhesives are conditioned at the
safety concerns, if any, associated with its use. It is the
adhesive manufacturer’s recommended application tempera-
responsibility of the user of this standard to establish appro-
ture for a conditioning cycle that corresponds to the expected
priate safety and health practices and determine the applica-
residence time during which the adhesive will be held molten
bility of regulatory limitations prior to use.
in the storage and application equipment. If so specified by the
adhesive manufacturer, the molten adhesive will be protected
2. Referenced Documents
against exposure to air.The total residence time is divided into
2
two or three intervals at which points the aged adhesive color
2.1 ASTM Standards:
and melt viscosity are measured and compared to the initial
D907Terminology of Adhesives
adhesive color and viscosity. Prior to measuring the melt
D1544TestMethodforColorofTransparentLiquids(Gard-
viscosity and color, the adhesive is subjectively evaluated for
ner Color Scale)
evidence of phase separation and surface skinning. Separate
D3236Test Method for Apparent Viscosity of Hot Melt
adhesive samples are conditioned for each test period.
Adhesives and Coating Materials
E691Practice for Conducting an Interlaboratory Study to
4.2 Thetestreportincludespercentchangeinmeltviscosity,
Determine the Precision of a Test Method
percentofadhesivesurfaceskinned,percentchangeinGardner
color, and description of phase separation, if any.
3. Terminology
5. Significance and Use
3.1 Definitions—Many of the terms found in this test
method are defined in Terminology D907.
5.1 Hot-melt adhesives must generally be applied at rela-
tively high temperatures in order that the adhesive viscosity is
3.2 Definitions of Terms Specific to This Standard:
low enough that it can be readily handled in typical hot-melt
3.2.1 color, n—the aspect of the appearance of an object
equipment. Changes in the adhesive caused by exposure to the
dependent upon the spectral composition of the incident light,
severe environment required during hot-melt processing will
the spectral reflectance or transmittance of the object, and the
disrupt the adhesive application process and may affect the
spectral response of an observer.
quality of the adhesive bond. Changes in adhesive viscosity
mayaffectthequantityofadhesivedispensedbytheapplicator.
Phase separation or changes in viscosity and color may be an
1
This test method is under the jurisdiction of ASTM Committee D10 on
indication of changes occurring in the adhesive which could
Packaging and is the direct responsibility of Subcommittee D10.14 on Tape and
Labels.
affect the quality of the adhesive joint. A skin formed on the
Current edition approved May 1, 2007. Published June 2007. Originally
adhesive may eventually clog the applicator nozzle or die.
approved in 1985. Last previous edition approved in 2000 as D4499–95(2000).
DOI: 10.1520/D4499-07.
5.2 The data generated in this test procedure are compara-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
tive in nature. Results can be useful in observing batch-to-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
batch variation or relative thermal stability of alternate adhe-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sive formulations. Results can also be useful in selecting
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4499 −
...

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5.1 These test methods provide a quantitative measure of the pressure-sensitive tack property of an adhesive.
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SCOPE
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5.1 When a box becomes wet, the performance of the box and its closure are reduced. It is desirable to have box closure methods that retain an ability to keep the box closed when wet. Sealing or reinforcing methods sometimes are useful to improve performance of wet boxes and closures. Water resistance is sometimes a regulatory or contractual requirement.  
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5.1 This test method measures the cohesive strength of the adhesive on a pressure sensitive article. The time to failure can predict end use properties of pressure sensitive articles such as edge ooze from cold flow; trimming, slitting and die cutting quality; telescoping in tapes; ability to seal packages; and vertical holding power.  
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SCOPE
1.1 This test method covers the ability of a pressure sensitive article (for example, tape, label, sticker, etc.) to remain adhered to a stainless steel panel under a constant load applied parallel to the bonding surface of the pressure sensitive article.  
1.2 Values stated in either SI or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents, therefore, each system must be used independently without combining values in any way.  
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