1、Designation: D4797 12aD4797 17Standard Test Methods forGravimetric Analysis of White and Yellow ThermoplasticTrafficPavement Marking1This standard is issued under the fixed designation D4797; the number immediately following the designation indicates the year oforiginal adoption or, in the case of r
2、evision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover procedures for the gravimetric analysis of the binder and hydrochloric A
3、cid (HCL) insolubleparticles in white and yellow thermoplastic trafficpavement 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 combinationof any two or more
4、 of these materials.1.2 This standard does not address the physical separation and the individual quantification of each component when a mixtureof two or more HCL insoluble materials is present. Rather it requires the user to visually evaluate the HCL insoluble material(obtained from following this
5、 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) whichis detailed in Test Methods D1394 and D126.1.4 This standard will attempt to address the interference of organic pigment
6、s with the binder results.1.5 The analytical procedures appear in the following order:SectionsPercent Binder 10Percent Retroreflective Optics orNon-Retroreflective Particles111.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information onl
7、y.1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations
8、 prior to use.1.8 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical
9、Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D126 Test Methods for Analysis of Yellow, Orange, and Green Pigments Containing Lead Chromate and Chromium OxideGreenD1394 Test Methods for Chemical Analysis of White Titanium PigmentsD7307 Practice for Sampling of Thermopl
10、astic Traffic Marking MaterialsD7308 Practice for Sample Preparation of Thermoplastic Pavement Marking MaterialsE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Terminology3.1
11、 Definitions of Terms Specific to This Standard: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 ofSubcommittee D01.44 on Traffic Coatings.Current edition approved Nov. 1, 2012Dec. 1, 20
12、17. Published December 2012February 2018. Originally approved in 1988. Last previous edition approved in 2012 asD4797 12.D4797 12a. DOI: 10.1520/D4797-12A.10.1520/D4797-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Ann
13、ual Book of ASTM Standardsvolume information, refer to the standardsstandards Document Summary page on the ASTM website.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. Becauseit m
14、ay 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 versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Har
15、bor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.1 ash, nthe inorganic components of thermoplastic trafficpavement marking including the pigment, glass spheres,retroreflective optics, and filler.3.1.2 binder, nthe organic components (resinous components) of thermoplastic t
16、rafficpavement marking that bind thepigments, glass spheres,retroreflective optics, and filler together as a unit.3.1.3 filler, nthe inorganic components of thermoplastic trafficpavement marking not including the pigments, retroreflectiveoptics, or non-retroreflective particles that are considered f
17、unctional.3.1.4 retroreflective optic, nfunctional particle that reflects and returns a relatively high proportion of light in a direction closeto the light source. This characteristic is maintained over a wide variation of the angle made by the incident light ray and normalto the retroreflective su
18、rface. This includes a single component structure such as a spherical glass bead or a multi componentstructure withcomposite optic such as a core andwith a surface covered with a small retroreflector.by small reflectors or such asa cluster of small reflectors bonded together.3.1.5 non-retroreflectiv
19、e particles, nfunctional particle that is insoluble in HCL, such as aluminum oxide, ground glass,quartz, etc., that are added for skid resistance or other non-retroreflective functional purpose.3.1.6 pigment, ntitanium dioxide, lead chromate colorants, and/or organic pigments.other inorganic or orga
20、nic pigments, orcombinations thereof.3.1.7 thermoplastic, nSee thermoplastic traffcpavement marking.3.1.8 thermoplastic traffcpavement marking, na highly filled 100 % total solids highway marking system that when heatedto a molten state can be extruded or sprayed onto a road surface and when cooled
21、forms a solid durable delineator.3.1.9 hydrochloric acid (HCL) insoluble particles, nretroreflective optics, such as glass beads or some other type ofretroreflective optic, or non-retroreflective particles such as silica sand, or a combination of any two or more of these materials.4. Summary of Test
22、 Method4.1 Thermoplastic trafficpavement marking material is prepared for the described test methods by melting a sample to itsapplication temperature under continuous agitation. The specimen is then poured into round patties on a non-stick surface such asa baking pan. The patties are then broken in
23、to pieces for ignition in a muffle furnace. The percent binder is calculated from theashed specimen and the specimen. The various tests for retroreflective optics, non-retroreflective particles, titanium dioxide, andlead chromate pigment can be performed later on the ashed residue. Determining the b
24、inder content of organic pigment containingthermoplastic may not be as straight forward. Specimen selection and preparation are the same for eacheither sample tested.type.5. Significance and Use5.1 The function of these test methods is to define the percent of binder and retroreflective optics or no
25、n-retroreflective particlesin the composition of the thermoplastic trafficpavement marking as defined by the applicable specification for the manufacture ofa specific thermoplastic trafficpavement marking. The subsequent sample, as a result of ashing can be used to later test for thepresence of tita
26、nium dioxide, lead chromate and possibly organic pigments.6. Apparatus6.1 Balance, analytical, capable of weighing to 0.1 mg.6.2 Crucibles, 30+ mL, porcelain or aluminum pan. (WarningSome aluminum pans will degrade at high temperatures.)6.3 Desiccator.6.4 Furnace (Muffle), capable of maintaining 540
27、C (1004F).6.5 Hot Plate or Heating Mantle, capable of heating a can of thermoplastic to 218C (425F).6.6 Sieve, 3 in., 45-m (No. 325) (metal).6.7 Buchner Funnel.6.8 Vacuum Flask and Rubber Hose.6.9 Vacuum Pump.6.10 Oven capable of reaching 218C (425F).6.11 Microwave Oven.6.12 400 mL Beaker or acid pr
28、oof container.6.13 Magnetic Stirring Bar.6.14 Magnetic Stirring Plate.6.15 Spatula.D4797 1726.16 Glass Beaker or Plastic Cup.7. Reagents7.1 Hydrochloric Acid Solution (HCL) (1 + 1 concentrated HCL diluted with equal volume of water).7.2 Hydrochloric Acid, Concentrated (HCL).8. Sampling8.1 Samples ma
29、y be obtained in accordance with Practice D7307 by an appropriate quartering or riffle sampling method wheredeemed necessary considering the physical form of the material.9. Preparation of Specimens9.1 Melt a sample of thermoplastic trafficpavement marking in accordance with Test Method Practice D73
30、08 to 218C (425F)(or per manufacturers recommended processing temperature) under continuous agitation on a hot plate or stir every 15 min in anoven set at 218C (425F) or per manufacturesmanufacturers recommended processing temperature.NOTE 1Road Thermoplastic pavement marking thermoplastic is manufa
31、ctured in a wide variety of viscosities at 218C. Some viscosities are so lowthat the retroreflective optics settle quickly. In order to prevent any settlement during the sampling process, removing the test sample at a lowertemperature is warranted. Some thermoplastic test samples are best poured as
32、low as 160C (320F) as long as they can flow into patties.9.2 Flow the sample out on a smooth clean non-stick surface and allow it to cool to room temperature. Patties approximately3 mm (18 in.) thick are usually easy to break upinto specimens for the described analysis.9.3 Break the specimen into sm
33、all pieces and weigh to the nearest 0.1 mg into a weighed crucible that is at least twice thevolume of specimen. The binder test can be done on samples as small as 10 g (0.353 g) and be effective. Larger samples can supplymore retroreflective optics or non-retroreflective particles for their evaluat
34、ion later if required.9.4 Cover the crucible and place into a muffle furnace preheated to 540C (1004F) and ash for 1 hour or until no carbonaceousmaterial remains.9.5 Remove the cruciblecrucible/pan with the ashed remains of the specimen and place into a desiccator and cool to roomtemperature.10. Pe
35、rcent Binder10.1 InterferencesIf yellow organic-pigment-containing road marking thermoplasticthermoplastic pavement marking samplesare ashed, the organic pigment may begin to degrade; therefore increasing the binder results. If the theoretical amount of organicpigment content of the sample is known
36、and an assumption can be made as to whether some or all the organic pigment hasdegraded (depending on its degradation temperature), temperature and the amount of filler in the pigment), then that amount canbe accounted for in the calculation in Eq 1.10.2 ProcedureWeigh the crucible and ash (see Sect
37、ion 9) to the nearest 0.1 mg and calculate the percent binder D as follows:D 51 2 S W! 3 100 (1)where:S = ashed weight of thermoplastic specimen, g, (crucible + ash wt.) crucible wt.W = weight of thermoplastic specimen, g, (crucible + thermoplastic specimen) crucible wt.where:S = ashed weight of the
38、rmoplastic specimen, g, (crucible + ash wt.) crucible wt.W = weight of thermoplastic specimen, g, (crucible + thermoplastic specimen) crucible wt.11. Percent Retroreflective Optics (RO) or Non-retroreflective Particles (NRP) using Hydrochloric Acid (HCL)11.1 Procedure:11.1.1 Weigh the crucible and a
39、sh (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 400-mL beaker or other acid-proof container and withminimal pressure, break apart the ashed specimen without crushing the retroreflective optics.11.1.3 Add to the ash ap
40、proximately 50 to 150 mL (1.7 to 5 oz.) of cold 1 + 1 HCL and stir occasionally until most of theeffervescence has ceased. (WarningThis is best performed under a vented hood. Also, this procedure can be performed usingwarmed HCL but is not necessary.)11.1.4 Immediately Once the solution has stopped
41、effervescing, dilute the contents with as much water as possible to allow theRO or NRP to settle. Decant the water and particulate carefully so as not to lose RO or NRP.11.1.5 If all the ash residue has not gone into solution, reintroduce HCL solution and stir. Continuous agitation can best beachiev
42、ed with a magnetic stirring bar and magnetic stirrer. Stirring with a spatula can achieve similar results.D4797 17311.1.6 Continue adding HCL or diluting with water and decanting until the water is clear.only beads and clear water are left inthe cup/beaker.11.1.7 Then transfer Transfer the residue i
43、nto a weighed 3-in. 45-m (No. 325) sieve or a Buchner funnel containing a weighedcorrugated coffee filter and wash with enough cold water to remove any residue. If the RO or NRPdo not appear clean, you shouldthen repeat the acid washing process.11.1.8 Dry the sides and the bottom of the sieve with a
44、 paper towel and dry for 1 hour in a gravity oven preheated to 100C(212F). If using a Buchner funnel and coffee filters, a vacuum can be pulled on the system to evacuate the water and then theRO/NRP-containing-filters can be dried in a oven or microwave oven.11.1.9 Place the sieve or coffee filter i
45、n a desiccator and cool to room temperature.11.1.10 Weigh the sieve/filter and HCLinsoluble particles (RO or NRP) to 0.1 mg and calculate the percent as follows (see Note2):NOTE 2Most road marking thermoplastic-ashed-residue thermoplastic pavement marking ashed residue which is insoluble in HCL is a
46、 retroreflectiveoptic.%HCL Insoluble Particles 5R/W! 3100 (2)where:R = weight of residue after acid wash (g) (not including sieve/filter wt.)W = original weight of thermoplastic specimen (g) (not including crucible wt.)11.1.11 After completing the calculation examine the sample of acid insoluble par
47、ticles obtained during the test to determinethe qualitative composition of the material. Include in the report the qualitative composition of the residue. For example, the HCLinsoluble particles obtained from this test are composed of 100 % retroreflective optics, or the HCL insoluble particles obta
48、inedfrom this test are composed of both retroreflective optics and non-retroreflective particles.12. Precision and Bias312.1 The precision of this test method is based on an interlaboratory study of ASTM D479712, Standard Test Methods forGravimetric Analysis of White and Yellow Thermoplastic Traffic
49、 Marking, conducted in 2012. Seven laboratories participated inthe study, testing four different thermoplastic materials. Every analyst was instructed to report four replicate test results in thisstudy. Practice E691 was followed for the study design; the details are given in ASTM Research Report No. RR:D01-1166.12.1.1 Repeatability Limit (r)Two test results obtained within one laboratory shall be judged not equivalent if they differ bymore than the “r” value for that material; “r” is the interval representing the critical
