ASTM D4797-17(2022)

Standard Test Methods for Gravimetric Analysis of White and Yellow Thermoplastic Pavement Marking

SIGNIFICANCE AND USE
5.1 The function of these test methods is to define the percent of binder and retroreflective optics or non-retroreflective particles in the composition of the thermoplastic pavement marking as defined by the applicable specification for the manufacture of a specific thermoplastic pavement marking. The subsequent sample, as a result of ashing can be used to later test for the presence of titanium dioxide, lead chromate and possibly organic pigments.
SCOPE
1.1 These test methods cover procedures for the gravimetric analysis of the binder and hydrochloric Acid (HCL) insoluble particles in white and yellow thermoplastic pavement markings. The HCL insoluble particles can be retroreflective optics, such as glass beads or some other type of retroreflective optic, or non-retroreflective particles such as silica sand, or a combination of any two or more of these materials.  
1.2 This standard does not address the physical separation and the individual quantification of each component when a mixture of two or more HCL insoluble materials is present. Rather it requires the user to visually evaluate the HCL insoluble material (obtained from following this test method) and report the types of materials present.  
1.3 This standard does not purport to address the titanium dioxide or lead chromate pigment measurement (after ashing) which is detailed in Test Methods D1394 and D126.  
1.4 This standard will attempt to address the interference of organic pigments with the binder results.  
1.5 The analytical procedures appear in the following order:    
Sections  
Percent Binder  
10  
Percent Retroreflective Optics or
Non-Retroreflective Particles  
11  
1.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.7 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.  
1.8 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: 93.080.30 - Road equipment and installations
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.44 - Traffic Coatings

Relations

• Refers: ASTM D1394-76(2020) - Standard Test Methods for Chemical Analysis of White Titanium Pigments
• Effective Date: 01-Jun-2020
• 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 D7308-07(2012) - Standard Practice for Sample Preparation of Thermoplastic Traffic Marking Materials
• Effective Date: 01-Jun-2012
• Refers: ASTM D126-87(2012) - Standard Test Methods for Analysis of Yellow, Orange, and Green Pigments Containing Lead Chromate and Chromium Oxide Green
• Effective Date: 01-Jun-2012
• 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 D1394-76(2009) - Standard Test Methods for Chemical Analysis of White Titanium Pigments
• 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 D7308-07 - Standard Practice for Sample Preparation of Thermoplastic Traffic Marking Materials
• Effective Date: 01-Jan-2007
• 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 D126-87(2006) - Standard Test Methods for Analysis of Yellow, Orange, and Green Pigments Containing Lead Chromate and Chromium Oxide Green
• Effective Date: 01-Nov-2006
• Refers: ASTM D7307-06 - Standard Practice for Sampling of Thermoplastic Traffic Marking Materials
• Effective Date: 01-Nov-2006

Overview

ASTM D4797-17(2022): Standard Test Methods for Gravimetric Analysis of White and Yellow Thermoplastic Pavement Marking provides precise procedures for determining the percent content of binder and hydrochloric acid (HCL) insoluble materials in thermoplastic pavement markings. Developed by ASTM International, this standard is critical for manufacturers, testing laboratories, and transportation agencies requiring quality control and material characterization for road marking products.

The standard outlines how to analyze white and yellow thermoplastic pavement markings by separating and quantifying the binder (organic resinous component) and the acid-insoluble particles, which include both retroreflective optics (such as glass beads) and non-retroreflective particles (such as silica sand). By following these test methods, users can assess compliance with material specifications, ensure product performance, and maintain roadway safety and visibility.

Key Topics

• Gravimetric Analysis Procedure
  The standard details the melting, ashing, acid-treatment, and weighing procedures required to determine binder content and identify acid-insoluble components in thermoplastic markings.

• Binder Content Determination
  Defines the test method for quantifying the percentage of binder remaining after ashing, which is essential for understanding the integrity and durability of pavement marking compounds.

• Assessment of Retroreflective and Non-Retroreflective Particles
  Covers identification and reporting processes for acid-insoluble materials, distinguishing between retroreflective optics (for nighttime visibility) and non-retroreflective fillers (for skid-resistance and body).

• Handling of Pigmented Samples
  Addresses potential interferences from organic and inorganic pigments, referencing additional ASTM methods (such as ASTM D1394 and D126) for more comprehensive pigment analysis.

• Reporting and Safety Considerations
  Emphasizes accurate visual identification and documentation of acid-insoluble material types, and mandates adherence to safety, health, and environmental best practices during testing.

Applications

• Quality Control in Manufacturing
  Ensures that thermoplastic pavement marking materials meet industry and regulatory requirements by accurately quantifying binder and functional mineral contents.

• Compliance Testing
  Supports conformance to contracts and governmental specifications for traffic safety products, especially those relating to road visibility and durability.

• Material Research and Development
  Provides a foundation for improving thermoplastic marking formulations by enabling detailed compositional analysis, supporting innovation in durable and high-performance markings.

• Performance Assessment
  Helps agencies evaluate pavement marking longevity and effectiveness, particularly with respect to retroreflectivity and resistance to weathering and traffic wear.

• Environmental and Safety Audits
  By referencing potential presence of substances such as lead chromate and titanium dioxide, this standard aids in regulatory compliance and environmental risk mitigation.

Related Standards

This standard references and complements several important ASTM documents:

• ASTM D126: Test Methods for Analysis of Yellow, Orange, and Green Pigments Containing Lead Chromate and Chromium Oxide Green
• ASTM D1394: Test Methods for Chemical Analysis of White Titanium Pigments
• ASTM D7307: Practice for Sampling of Thermoplastic Pavement Marking Materials
• ASTM D7308: Practice for Sample Preparation of Thermoplastic Pavement Marking Materials
• ASTM E177: Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• ASTM E691: Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method

For comprehensive testing and specification of thermoplastic pavement markings, users should consult these related standards in conjunction with ASTM D4797-17(2022).

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Keywords: ASTM D4797, thermoplastic pavement marking, gravimetric analysis, binder content, retroreflective optics, non-retroreflective particles, quality control, compliance testing, road marking materials, hydrochloric acid insoluble, ASTM standards, traffic safety products.

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: D4797 − 17 (Reapproved 2022)
Standard Test Methods for
Gravimetric Analysis of White and Yellow Thermoplastic
Pavement Marking
This standard is issued under the fixed designation D4797; 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 Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
1.1 These test methods cover procedures for the gravimetric
Barriers to Trade (TBT) Committee.
analysis of the binder and hydrochloric Acid (HCL) insoluble
particles in white and yellow thermoplastic pavement mark-
2. Referenced Documents
ings. The HCLinsoluble particles can be retroreflective optics,
2.1 ASTM Standards:
such as glass beads or some other type of retroreflective optic,
D126 Test Methods for Analysis of Yellow, Orange, and
or non-retroreflective particles such as silica sand, or a com-
Green Pigments Containing Lead Chromate and Chro-
bination of any two or more of these materials.
mium Oxide Green
1.2 This standard does not address the physical separation
D1394 Test Methods for Chemical Analysis of White Tita-
and the individual quantification of each component when a
nium Pigments
mixture of two or more HCL insoluble materials is present.
D7307 Practice for Sampling of Thermoplastic Pavement
Rather it requires the user to visually evaluate the HCL
Marking Materials
insoluble material (obtained from following this test method)
D7308 Practice for Sample Preparation of Thermoplastic
and report the types of materials present.
Pavement Marking Materials
1.3 This standard does not purport to address the titanium E177 Practice for Use of the Terms Precision and Bias in
dioxide or lead chromate pigment measurement (after ashing)
ASTM Test Methods
which is detailed in Test Methods D1394 and D126. E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.4 This standard will attempt to address the interference of
organic pigments with the binder results.
3. Terminology
1.5 The analytical procedures appear in the following order:
3.1 Definitions of Terms Specific to This Standard:
Sections
3.1.1 ash, n—the inorganic components of thermoplastic
Percent Binder 10
pavement marking including the pigment, retroreflective
Percent Retroreflective Optics or 11
Non-Retroreflective Particles
optics, and filler.
1.6 The values stated in SI units are to be regarded as the
3.1.2 binder, n—the organic components (resinous compo-
standard. The values given in parentheses are for information
nents) of thermoplastic pavement marking that bind the
only.
pigments, retroreflective optics, and filler together as a unit.
1.7 This standard does not purport to address all of the
3.1.3 filler, n—the inorganic components of thermoplastic
safety concerns, if any, associated with its use. It is the
pavement marking not including the pigments, retroreflective
responsibility of the user of this standard to establish appro-
optics, or non-retroreflective particles that are considered
priate safety, health, and environmental practices and deter-
functional.
mine the applicability of regulatory limitations prior to use.
3.1.4 retroreflective optic, n—functionalparticlethatreflects
1.8 This international standard was developed in accor-
and returns a relatively high proportion of light in a direction
dance with internationally recognized principles on standard-
close to the light source. This characteristic is maintained over
ization established in the Decision on Principles for the
a wide variation of the angle made by the incident light ray and
normal to the retroreflective surface. This includes a single
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 D01.44 on Traffic Coatings. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2022. Published December 2022. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1988. Last previous edition approved in 2017 as D4797 – 17. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4797-17R22. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4797 − 17 (2022)
component structure such as a spherical glass bead or a 6.5 HotPlateorHeatingMantle,capableofheatingacanof
composite optic such as a core with a surface covered by small thermoplastic to 218 °C (425 °F).
reflectors or such as a cluster of small reflectors bonded
6.6 Sieve, 3 in., 45 µm (No. 325) (metal).
together.
6.7 Buchner Funnel.
3.1.5 non-retroreflective particles, n—functional particle
6.8 Vacuum Flask and Rubber Hose.
that is insoluble in HCL, such as aluminum oxide, ground
glass, quartz, etc., that are added for skid resistance or other
6.9 Vacuum Pump.
non-retroreflective functional purpose.
6.10 Oven capable of reaching 218 °C (425 °F).
3.1.6 pigment, n—titanium dioxide, lead chromate
6.11 Microwave Oven.
colorants, other inorganic or organic pigments, or combina-
6.12 400 mL Beaker or acid proof container.
tions thereof.
3.1.7 thermoplastic, n—See thermoplastic pavement mark- 6.13 Magnetic Stirring Bar.
ing.
6.14 Magnetic Stirring Plate.
3.1.8 thermoplastic pavement marking, n—a highly filled
6.15 Spatula.
100 % total solids highway marking system that when heated
6.16 Glass Beaker or Plastic Cup.
toamoltenstatecanbeextrudedorsprayedontoaroadsurface
and when cooled forms a solid durable delineator.
7. Reagents
3.1.9 hydrochloric acid (HCL) insoluble particles,
7.1 Hydrochloric Acid Solution (HCL) (1 + 1 concentrated
n—retroreflective optics, such as glass beads or some other
HCL diluted with equal volume of water).
type of retroreflective optic, or non-retroreflective particles
7.2 Hydrochloric Acid, Concentrated (HCL).
such as silica sand, or a combination of any two or more of
these materials.
8. Sampling
4. Summary of Test Method
8.1 Samples may be obtained in accordance with Practice
D7307 by an appropriate quartering or riffle sampling method
4.1 Thermoplastic pavement marking material is prepared
where deemed necessary considering the physical form of the
for the described test methods by melting a sample to its
material.
application temperature under continuous agitation. The speci-
men is then poured into round patties on a non-stick surface
9. Preparation of Specimens
such as a baking pan. The patties are then broken into pieces
for ignition in a muffle furnace. The percent binder is calcu- 9.1 Melt a sample of thermoplastic pavement marking in
lated from the ashed specimen. The various tests for retrore-
accordance with Practice D7308 to 218 °C (425 °F) (or per
flective optics, non-retroreflective particles, titanium dioxide, manufacturers recommended processing temperature) under
andleadchromatepigmentcanbeperformedlaterontheashed
continuous agitation on a hot plate or stir every 15 min in an
residue. Determining the binder content of organic pigment oven set at 218 °C (425 °F) or per manufacturer’s recom-
containing thermoplastic may not be as straight forward.
mended processing temperature.
NOTE 1—Thermoplastic pavement marking is manufactured in a wide
Specimen selection and preparation are the same for either
variety of viscosities at 218 °C. Some viscosities are so low that the
sample type.
retroreflective optics settle quickly. In order to prevent any settlement
during the sampling process, removing the test sample at a lower
5. Significance and Use
temperatureiswarranted.Somethermoplastictestsamplesarebestpoured
as low as 160 °C (320 °F) as long as they can flow into patties.
5.1 The function of these test methods is to define the
percent of binder and retroreflective optics or non-
9.2 Flowthesampleoutonasmoothcleannon-sticksurface
retroreflective particles in the composition of the thermoplastic
andallowittocooltoroomtemperature.Pattiesapproximately
pavement marking as defined by the applicable specification
3mm( ⁄8in.)thickareusuallyeasytobreakintospecimensfor
for the manufacture of a specific thermoplastic pavement
the described analysis.
marking. The subsequent sample, as a result of ashing can be
9.3 Break the specimen into small pieces and weigh to the
used to later test for the presence of titanium dioxide, lead
nearest 0.1 mg into a weighed crucible that is at least twice the
chromate and possibly organic pigments.
volumeofspecimen.Thebindertestcanbedoneonsamplesas
small as 10 g (0.353 g) and be effective. Larger samples can
6. Apparatus
supply more retroreflective optics or non-retroreflective par-
6.1 Balance, analytical, capable of weighing to 0.1 mg.
ticles for their e
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