ASTM D4797-12
(Test Method)Standard Test Methods for Gravimetric Analysis of White and Yellow Thermoplastic Traffic Marking
Standard Test Methods for Gravimetric Analysis of White and Yellow Thermoplastic Traffic 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 traffic marking as defined by the applicable specification for the manufacture of a specific thermoplastic traffic 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 traffic 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D4797 − 12
StandardTest Methods for
Gravimetric Analysis of White and Yellow Thermoplastic
1
Traffic 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 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 These test methods cover procedures for the gravimetric
D126 Test Methods for Analysis of Yellow, Orange, and
analysis of the binder and hydrochloric Acid (HCL) insoluble
Green Pigments Containing Lead Chromate and Chro-
particles in white and yellow thermoplastic traffic markings.
mium Oxide Green
The HCL insoluble particles can be retroreflective optics, such
D1394 Test Methods for Chemical Analysis of White Tita-
as glass beads or some other type of retroreflective optic, or
nium Pigments
non-retroreflective particles such as silica sand, or a combina-
D7307 PracticeforSamplingofThermoplasticTrafficMark-
tion of any two or more of these materials.
ing Materials
1.2 This standard does not address the physical separation D7308 Practice for Sample Preparation of Thermoplastic
and the individual quantification of each component when a Traffic Marking Materials
mixture of two or more HCL insoluble materials is present.
3. Terminology
Rather it requires the user to visually evaluate the HCL
3.1 Definitions of Terms Specific to This Standard:
insoluble material (obtained from following this test method)
3.1.1 ash, n—the inorganic components of thermoplastic
and report the types of materials present.
traffic marking including the pigment, glass spheres, and filler.
1.3 This standard does not purport to address the titanium
3.1.2 binder, n—the organic components (resinous compo-
dioxide or lead chromate pigment measurement (after ashing)
nents) of thermoplastic traffic marking that bind the pigments,
which is detailed in Test Methods D1394 and D126.
glass spheres, and filler together as a unit.
1.4 This standard will attempt to address the interference of
3.1.3 filler, n—the inorganic components of thermoplastic
organic pigments with the binder results.
traffic marking not including the pigments, retroreflective
optics, or non-retroreflective particles that are considered
1.5 The analytical procedures appear in the following order:
functional.
Sections
3.1.4 retroreflective optic, n—functionalparticlethatreflects
Percent Binder 10
Percent Retroreflective Optics or 11
and returns a relatively high proportion of light in a direction
Non-Retroreflective Particles
close to the light source. This characteristic is maintained over
1.6 The values stated in SI units are to be regarded as the a wide variation of the angle made by the incident light ray and
standard. The values given in parentheses are for information normal to the retroreflective surface. This includes a single
component structure such as a spherical glass bead or a multi
only.
component structure with a core and a surface covered with a
1.7 This standard does not purport to address all of the
small retroreflector.
safety concerns, if any, associated with its use. It is the
3.1.5 non-retroreflective particles, n—functional particle
responsibility of the user of this standard to establish appro-
that is insoluble in HCL, such as aluminum oxide, ground
priate safety and health practices and determine the applica-
glass, quartz, etc., that are added for skid resistance or other
bility of regulatory limitations prior to use.
non-retroreflective functional purpose.
3.1.6 pigment, n—titanium dioxide, lead chromate
colorants, and/or organic pigments.
1
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct
2
responsibility of Subcommittee D01.44 on Traffic Coatings. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved June 1, 2012. Published August 2012. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1988. Last previous edition approved in 2007 as D4797 – 88 (2007). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D4797-12. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D4797 − 12
3.1.7 thermoplastic, n—See thermoplastic traffıc marking. 7. Reagents
3.1.8 thermoplastic traffıc marking, n—a highly filled
7.1 Hydrochloric Acid Solution (HCL) (1 + 1 concentrated
100 % total solids highway marking system that when heated
HCL
...
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: D4797 − 88 (Reapproved 2007) D4797 − 12
Standard Test Methods for
Chemical and Gravimetric Analysis of White and Yellow
Thermoplastic Traffic Marking Containing Lead Chromate
1
and Titanium Dioxide
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
1.1 These test methods cover procedures for the chemical and gravimetric analysis of the binder and hydrochloric Acid (HCL)
insoluble particles in white and yellow thermoplastic traffic marking containing lead chromate and titanium dioxide pigment.
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:
1
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.
Current edition approved Nov. 1, 2007June 1, 2012. Published November 2007August 2012. Originally approved in 1988. Last previous edition approved in 20042007
as D4797 – 88 (2004).D4797 – 88 (2007). DOI: 10.1520/D4797-88R07.10.1520/D4797-12.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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D4797 − 12
Sections
Percent Binder 10
Percent Glass Beads (Note 1 11
)
Percent Retroreflective Optics or 11
Non-Retroreflective Particles
Percent Titanium Dioxide 12
Percent Lead Chromate and Analysis of Chrome Yellow and 13
Chrome Orange Pigments (Note 2)
2
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D4797 − 12
Weigh the crucible and ash (see Section 9) to the nearest 0.1 mg and calculate the percent binder D as follows:
D 5 (12 (S⁄W)) 3 100 (1)
3
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D4797 − 12
where:
S = ashed weight of thermoplastic specimen, g, (crucible + ash wt.) – crucible wt.
W = weight of thermoplastic specimen, g, (crucible + thermoplastic specimen) – crucible wt.
11. Percent Glass Beads Retroreflective Optics (RO) or Non-retroreflective Particles (NRP) using Hydrochloric Acid
(HCL)
11.1 Interferences—Acid-insoluble fillers will affect the glass-sphere analysis and must be removed by some physical separation
method or accounted for quantitatively, or both.
11.1 Procedure:
11.1.1 Weigh the crucible and ash (see Section 9) to 0.1 mg and calculate the percent ash.
11.1.2 After the ashed material has been weighed, transfer the ash to a mortar and pestle and grind with minimal pressure to
reduce the ash to a fine grained consistency 400-mL beaker or other acid-proof container and with minimal pressure, break apart
the ashed specimen without crushing the beads. Carefully transfer the ashed contents into a 400-mL beaker.retroreflective optics.
11.1.3 Add to the ash approximately 50 to 150 mL (1.7 to 5 oz.) of cold 1 + 2 HCl1 + 1 HCL and stir occasionally until most
of the effervescence has ceasedceased. completely.(Warning—This is best performed under a vented hood. Also, this procedure
can be performed using warmed HCL but is not necessary.)
11.2.4 Place the beaker on a hot plate preheated to approximately 260°C and boil for 20 min under continuous agitation to
dissolve all acid-soluble filler pigments.
11.1.4 Remove the beaker from the hot plate, and while hot, immediately Immediately dilute the contents with 150 mL of cold
water. Allow the beads as much water as possible to allow the RO or NRP to settle. Decant the wate
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