1、Designation: D 4451 02Standard 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 year of last revision
2、. 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 pre-formed tape) by
3、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 of this standard
4、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:D 3723 Test Method for Pigment Content of Water-Emulsion Paints by Low-Temperature Ashing2E 180 Practice for Determining the Precisi
5、on of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals33. 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 heated at450C. The d
6、ish 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. Reagents5.1 Puri
7、ty 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.45.2 Toluene.6. Procedure
8、6.1 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-mL syringe and weigh to 0.1 mg. Transfer about 5 mLtoluene to a porcelain dish t
9、ared 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 possibleover a meker burn
10、er 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 Tape Cut about a 10-gsquare of the product. Remove the adhesive by pulling it off orby using an appropriate solvent. Save the beads tha
11、t 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 in a furnace hoo
12、d untilthe material catches fire. Do not leave the dish on the burnerafter the flame has subsided. Transfer to the muffle furnace andproceed as in 6.4.6.3 Thermoplastic Traffc Marking MaterialThis materialmay be delivered in block or powdered form. Transfer about400 g of the sample to a quart contai
13、ner and heat in a forceddraft oven at 400F until completely melted (may 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 101This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatin
14、gs, Materials, and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved Jan. 10, 2002. Published March 2002. Originallypublished as D 4451 - 85. Last previous edition D 4451 - 85 (1996).2Annual Book of ASTM St
15、andards, Vol 06.01.3Annual Book of ASTM Standards, Vol 15.05.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BD
16、H Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.g wafer from the aluminum dish and weigh
17、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 until 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
18、 muffle furnace in a fumehood at 450C (see Test Method D 3723). Heat overnight oruntil no further carbonaceous material is 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,
19、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 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 interlaborator
20、ystudy in which one operator in 7 different laboratories analyzedin duplicate on two days six samples of commercial wholepaint or thermoplastic material containing 50 to 80 % pigment.The results were analyzed statistically in accordance withPractice E 180 and the within-laboratory coefficient of var
21、ia-tion was found to be 0.10 % relative at 36 df and thebetween-laboratories coefficient of variation 0.25 % relative at30 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 th
22、e mean of dupli-cate determinations, obtained by the same operator on differentdays should be considered suspect if they differ 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 conside
23、red suspect if they differ by more than0.72 % relative.9. Bias9.1 Bias cannot be determined because there are no stan-dards for pigment content of paints.10. Keywords10.1 ignition; low temperature ashing; pigment; pigmentcontent of paintsASTM International takes no position respecting the validity o
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27、opyrighted 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 44512
