1、Designation: D 4797 88 (Reapproved 2007)Standard Test Methods forChemical and Gravimetric Analysis of White and YellowThermoplastic Traffic Marking Containing Lead Chromateand Titanium Dioxide1This standard is issued under the fixed designation D 4797; the number immediately following the designatio
2、n indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover procedures
3、 for the chemicaland gravimetric analysis of white and yellow thermoplastictraffic marking containing lead chromate and titanium dioxidepigment.1.2 The analytical procedures appear in the following order:SectionsPercent Binder 10Percent Glass Beads (Note 1) 11Percent Titanium Dioxide 12Percent Lead
4、Chromate and Analysis of Chrome Yellow andChrome Orange Pigments (Note 2)131.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its
5、 use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.NOTE 1Test for 1.50 glass spheres only.NOTE 2This modified analysis of chrome yellow and chrome orangepigments must
6、 be used because the heat resistant chrome yellows in thethermoplastic cannot be analyzed by Test Methods D 126.2. Referenced Documents2.1 ASTM Standards:2D 126 Test Methods for Analysis of Yellow, Orange, andGreen Pigments Containing Lead Chromate and Chro-mium Oxide GreenD 883 Terminology Relating
7、 to PlasticsD 1193 Specification for Reagent WaterD 1394 Test Methods for Chemical Analysis of WhiteTitanium PigmentsF 412 Terminology Relating to Plastic Piping Systems3. Terminology3.1 DefinitionsDefinitions are in accordance with Termi-nology D 883 and F 412, unless otherwise indicated.3.2 Defini
8、tions of Terms Specific to This Standard:3.2.1 ash, nthe inorganic components of thermoplastictraffic marking including the pigment, glass spheres, and filler.3.2.2 binder, nthe organic components of thermoplastictraffic marking that bind the pigments, glass spheres, and fillertogether as a unit.3.2
9、.3 filler, nthe inorganic components of thermoplastictraffic marking not including the pigments or glass spheres.3.2.4 pigment, ntitanium dioxide and lead chromate colo-rants.3.2.5 thermoplastic, nSee thermoplastic traffc marking.3.2.6 thermoplastic traffc marking, na highly filled100 % total solids
10、 highway marking system that when heatedto a molten state can be extruded or sprayed onto a road surfaceand when cooled forms a solid durable delineator.4. Summary of Test Method4.1 The thermoplastic material is prepared for the describedtest methods by melting a sample to its application temperatur
11、eunder continuous agitation. The specimen is then poured intoround patties on a clean tin plate or baking pan. The patties arethen broken into pieces for ignition in a muffle furnace. Thepercent binder is calculated from the ashed specimen and thevarious tests for glass spheres, titanium dioxide, an
12、d leadchromate pigment are performed on the ashed residue. Thetests for pigment type or glass spheres may be run on the sameashed specimen. Specimen selection and preparation are thesame for each sample tested.5. Significance and Use5.1 The function of these test methods is to define thepercent of b
13、inder, glass, titanium dioxide, and lead chromatepresent in the composition of the thermoplastic traffic marking1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.44 on Tr
14、affic Coatings.Current edition approved Nov. 1, 2007. Published November 2007. Originallyapproved in 1988. Last previous edition approved in 2004 as D 4797 88 (2004).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual B
15、ook of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.as defined by the applicable specification for the manufactureof a specific ther
16、moplastic traffic marking.6. Apparatus6.1 Balance, analytical, accurate to 0.1 mg.6.2 Buret, 10 mL, 0.1-mL divisions.6.3 Buret, 50 mL, 0.1-mL divisions.6.4 Crucibles, 30 mL, porcelain.6.5 Desiccator.6.6 Erlenmeyer flask, 500 mL.6.7 Furnace (Muffle), capable of maintaining 1100C.6.8 Hot Plate, capabl
17、e of maintaining 537C.6.9 Jones Reductor.6.10 Mortar and Pestle, glazed ceramic or other impervioustype.6.11 Oven, capable of maintaining 260C.6.12 Sieve, 3 in., 45-m (No. 325) (metal).7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it
18、is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its u
19、se without lessening theaccuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type IV of Specification D 1193.7.3 AlcoholEthyl alcohol 95 %.7.4 Potassium Chloride (KCl).7.5 Potassium Hydroxide SolutionDi
20、ssolve 50 g of potas-sium hydroxide (KOH) in 100 mL of freshly distilled water.7.6 Potassium Iodide (KI).7.7 Potassium Permanganate Solution (KMnO4) (0.1N).7.8 Sodium Thiosulfate, Standard Solution(NA2S2O35H2O) (0.1 N).7.9 Starch (Soluble) Indicator SolutionDissolve 10 g ofsoluble starch in 1 L of d
21、eionized or distilled water.7.10 Hydrochloric Acid Solution (HCl) (1 + 2).7.11 Hydrochloric Acid, Concentrated (HCl).8. Sampling8.1 Samples may be obtained by an appropriate quarteringor riffle sampling method where deemed necessary consideringthe physical form of the material.9. Preparation of Spec
22、imens9.1 Melt a sample of approximately 1000 g of thermoplastictraffic marking to 210 to 218C under continuous agitation ona hot plate set at 537C or stir every 15 min in an oven set at260C.9.2 Flow the sample out on a smooth clean surface andallow it to cool to room temperature. Patties 3 mm (18 in
23、.) thickwill facilitate breaking up specimens for the described analysis.9.3 Break the specimen into small pieces and weigh 10 g tothe nearest 0.1 mg into a 30-mL weighed crucible.9.4 Cover the crucible and place into a muffle furnacepreheated to 540C and ash for1horuntil no carbonaceousmaterials re
24、main.9.5 Remove the crucible with the ashed remains of thespecimen and place into a desiccator and cool to roomtemperature.10. Percent Binder10.1 Procedure:10.1.1 Weigh the crucible and ash (see Section 9)tothenearest 0.1 mg and calculate the percent of organic binder D asfollows:D 5 1 2 S/W!# 3 100
25、 (1)where:S = ashed weight of thermoplastic specimen, g, andW = weight of thermoplastic specimen, g.11. Percent Glass Beads11.1 InterferencesAcid-insoluble fillers will affect theglass-sphere analysis and must be removed by some physicalseparation method or accounted for quantitatively, or both.11.2
26、 Procedure:11.2.1 Weigh the crucible and ash (see Section 9) to 0.1 mgand calculate the percent ash.11.2.2 After the ashed material has been weighed, transferthe ash to a mortar and pestle and grind with minimal pressureto reduce the ash to a fine grained consistency without crushingthe beads. Caref
27、ully transfer the ashed contents into a 400-mLbeaker.11.2.3 Add to the ash approximately 150 mL of cold 1 + 2HCl and stir occasionally until the effervescence has ceasedcompletely.11.2.4 Place the beaker on a hot plate preheated to approxi-mately 260C and boil for 20 min under continuous agitation t
28、odissolve all acid-soluble filler pigments.11.2.5 Remove the beaker from the hot plate, and while hot,immediately dilute the contents with 150 mL of cold water.Allow the beads to settle. Decant the water carefully so as notto lose any glass beads.11.2.6 Continue diluting with 150-mL aliquots of wate
29、r anddecanting until the water is nearly clear. Then transfer theresidue into a weighed 3-in. 45-m (No. 325) sieve and washwith 500 mL of cold water.11.2.7 Dry the sides and the bottom of the sieve with a papertowel and dry for1hinagravity oven preheated to 100C.11.2.8 Place the sieve in a desiccato
30、r and cool to roomtemperature. Weigh the sieve and glass beads to 0.1 mg andcalculate the percent beads G as follows:3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical S
31、ociety, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D 4797 88 (2007)2G 5 B/W! 3 100 (2)where:B = weight of the glass beads, g, andW = weight of thermopl
32、astic specimen, g.12. Percent Titanium Dioxide12.1 Procedure:12.1.1 Weigh the crucible and ash (see Section 9) to 0.1 mgand calculate the percent of ash which is also equal to thepercent filler (pigments and beads).12.1.2 After weighing the above ashed materials, carefullytransfer the ash to an agat
33、e or similar impervious-type mortar.Grind the ash to a consistent fine powder except for the glassbeads. The pulverized ash must be stirred each time specimensare taken to weigh the prescribed amount for the analysis.12.1.3 Weigh 1 6 0.1 g of ash for the titanium analysis.12.1.4 Proceed with the tit
34、anium analysis as described inTest Methods D 1394. The Jones Reductor or aluminumreduction method may be used.12.1.5 At the end of the digestions described in TestMethods D 1394, filter the undigested materials through a 3-in.45-m (No. 325) sieve with hot water. This will preventclogging of the Jone
35、s Reductor. This step is not necessary if thealuminum reduction method is used.12.1.6 Calculate the percent of titanium dioxide (TiO2) fromthe total ash weighed. The result gives the percent of TiO2inthe total thermoplastic specimen.12.1.7 Calculate the percent ash A as follows:A 5 S/W! 3 100 (3)whe
36、re:S = weight of ash, g, andW = weight of thermoplastic specimen used, g.12.1.8 Calculate the percent of total TiO2in the T based onpercent ash:T 5 0.08 AMN/CSa(4)where:A = ash (pigment + filler + beads), %,Sa= weight of ash used, g,M = amount of 0.1 N potassium permanganate (KMnO4)solution used, mL
37、, (see the paragraph on titrationwith KMnO4solution of the Procedure section ofthe Jones Reductor Method of Test MethodsD 1394),N = normality of KMnO4used,C = correction factor for TiO2pigment used (usually1.0). This represents the purity of the pigment ifspecified, and0.08 = weight of TiO2per1mLof1
38、N KMnO4,g.13. Percent Lead Chromate13.1 Procedure:13.1.1 Weigh the crucible and ash (see Section 9) to 0.1 mgand calculate the percent of ash.13.1.2 After weighing the above ashed materials, carefullytransfer the ash to an agate or similar impervious type mortarand grind the ash to a consistent fine
39、 powder except for theglass beads. The pulverized ash must be stirred when speci-mens are taken to weigh the prescribed amount for the analysis.13.1.3 Weigh 1 6 0.1 g of the ash for the lead chromate(PbCrO4) analysis.13.1.4 Analyze the dry ash as follows:13.1.4.1 Transfer the ashed specimen to a 500
40、-mL Erlenm-eyer flask. Add 6 mL of the (KOH) solution (see 7.5) and 10mL of distilled water. Heat until dissolved. Do not allow to dry.To the hot solution add 50 g of KCl. Dilute with water to 200mL and swirl until dissolved. Add 16 mL of HCl slowly. Add10 g of KI and titrate with the standard sodiu
41、m thiosulfatesolution (see 7.7) using the starch solution (see 7.8)astheindicator. Titrate to a green endpoint.NOTE 3A 10-mL buret may be used since the titrant required is smallfor most thermoplastic analysis.13.1.5 Calculate the percent ash A as follows:A 5 S/W! 3 100 (5)where:S = weight of gas, g
42、, andW = weight of the thermoplastic specimen used, g.13.1.6 Calculate the percent of total PbCrO4in the sample(binder + filler) L based on percent ash as follows:L 5 0.1077 AMN/CSa(6)where:A = ash (pigment + filler + beads), %,C = correction factor for PbCrO4pigment used (for ex-ample, 90 to 100 %,
43、 normally 1.0). This representsthe purity of the pigment if specified,M = amount of 0.1 N sodium thiosulfate solution used,mL,N = normality of sodium thiosulfate used, andSa= weight of ash used, g.14. Precision and Bias14.1 No general statement of precision can be made becauseof lack of sufficient d
44、ata at this time.14.2 No statement of bias can be prepared for this testmethod since there is no absolute method for use as a basis forcomparison.15. Keywords15.1 glass spheres (in traffic paint); lead chromate; titaniumdioxide; thermoplastic traffic marking materialD 4797 88 (2007)3ASTM Internation
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48、 at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 4797 88 (2007)4
