1、Designation: D 4451 02 (Reapproved 2008)Standard Test Method forPigment Content of Paints by Low-Temperature Ashing1This standard is issued under the fixed designation D 4451; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r 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 This test method covers the pigment content of paintsand several traffic marking materials (thermoplastic and pr
3、e-formed tape) by low-temperature furnace ashing. Some organicpigments may be lost by this method and some water ormoisture contained in pigments will be lost.1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user
4、 of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 3723 Test Method for Pigment Content of Water-Emulsion Paints by Low-Temperature AshingE 180 Practice for Deter
5、mining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals3. Summary of Test Method3.1 The specimen is transferred to a tared porcelain dish,dried (if necessary) at 105C, and heated on a burner. The dishand specimen are transferred to a muffle furnace and hea
6、ted at450C. The dish and specimen are reweighed and the pigment(ash) content calculated.4. Apparatus4.1 Muffle Furnace, maintained at 450C 6 25C.4.2 Circulating Oven, maintained at 105C 6 2C.4.3 Porcelain Dishes, 90-mm diameter.4.4 Plastic Disposable Syringe, 10-mL capacity.4.5 Burner, meker type.5.
7、 Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it 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.35.2 Tol
8、uene.6. Procedure6.1 Liquid-Paint:6.1.1 Mix the sample until homogeneous, preferably on amechanical shaker. If air bubbles become entrapped in thepaint, stir it by hand.6.1.2 Draw slightly more than 10 g of the paint under testinto a 10-mLsyringe and weigh to 0.1 mg. Transfer about 5 mLtoluene to a
9、porcelain dish tared with a paper clip for use as astirrer. Add 10 g of the material into the toluene. Reweigh thesyringe to 0.1 mg and calculate the specimen weight. Mix wellon a magnetic stirrer. Place the dish in the oven at 105C for 30min.6.1.3 Remove and heat at the lowest temperature possibleo
10、ver a meker burner in a fume hood. Do not leave the dish onthe burner after the flame has subsided. Transfer to the mufflefurnace and proceed as in 6.4.6.2 Preformed Traffc Marking TapeCut about a 10-gsquare of the product. Remove the adhesive by pulling it off orby using an appropriate solvent. Sav
11、e the beads that areknocked off by this process and weigh with the tape. Dry thespecimen for 30 min at 105C to remove the solvent. Cool ina desiccator. Weigh the specimen along with the loose beads to0.1 mg into a tared porcelain dish. Heat in a fume hood at thelowest temperature of a meker burner i
12、n a furnace hood untilthe material catches fire. Do not leave the dish on the burnerafter the flame has subsided. Transfer to the muffle furnace andproceed as in 6.4.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the
13、 direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved Feb. 1, 2008. Published February 2008. Originallyapproved in 1985. Last previous edition approved in 2002 as D 4451 - 02.2For referenced ASTM standards, visit the ASTM website, ww
14、w.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions
15、 on the testing of reagents notlisted by the American Chemical Society, 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.1Copyright ASTM International, 100 B
16、arr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.3 Thermoplastic Traffc Marking MaterialThis materialmay be delivered in block or powdered form. Transfer about400 g of the sample to a quart container and heat in a forceddraft oven at 400F until completely melted (may
17、take as longas 4 h). Stir vigorously until well mixed. Pour about 10 g of thesample into an aluminum dish and let it cool. Remove the 10g wafer from the aluminum dish and weigh to 0.1 mg. Transferto a tared porcelain dish. Heat the dish at the lowest tempera-ture of a meker burner in a fume hood unt
18、il the specimencatches fire. Do not leave the dish on the burner after the flamehas subsided. Transfer to a muffle furnace and proceed as in6.4.6.4 Place the porcelain dish in a muffle furnace in a fumehood at 450C (see Test Method D 3723). Heat overnight oruntil no further carbonaceous material is
19、noted. Cool in adesiccator and reweigh the dish plus the residue to 0.1 mg.Calculate the residue as percent pigment or, in the case ofthermoplastic material and preformed tape, as pigment andbeads.7. Calculation7.1 Calculate the percent pigment, P, as follows:P 5 C 2 A/S 3 100 (1)where:C = weight of
20、 dish and specimen after ignition in furnace,g,A = weight of dish alone, g, andS = specimen weight used, g.8. Precision8.1 The precision estimates are based on an interlaboratorystudy in which one operator in 7 different laboratories analyzedin duplicate on two days six samples of commercial wholepa
21、int or thermoplastic material containing 50 to 80 % pigment.The results were analyzed statistically in accordance withPractice E 180 and the within-laboratory coefficient of varia-tion was found to be 0.10 % relative at 36 df and thebetween-laboratories coefficient of variation 0.25 % relative at30
22、df. Based on these coefficients the following criteria shouldbe used for judging the acceptability of results at the 95 %confidence level:8.1.1 RepeatabilityTwo results, each the mean of dupli-cate determinations, obtained by the same operator on differentdays should be considered suspect if they di
23、ffer by more than0.28 % relative.8.1.2 ReproducibilityTwo results, each the mean of dupli-cate determinations, obtained by operators in different labora-tories should be considered suspect if they differ by more than0.72 % relative.9. Bias9.1 Bias cannot be determined because there are no stan-dards
24、 for pigment content of paints.10. Keywords10.1 ignition; low temperature ashing; pigment; pigmentcontent of paintsASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly ad
25、vised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, eithe
26、r reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend.
27、If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, 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 4451 02 (2008)2
