1、Designation:D30584(Reapproved 2014)Standard Test Method forSolvent-Extractable Material in Black Pigments1This standard is issued under the fixed designation D305;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revis
2、ion.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S.Department of Defense.1.Scope1.1 This test method covers the determination of the
3、solvent-extractable material in black pigments such as carbonblack,lampblack,and bone black.1.2 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns,if any,assoc
4、iated with its 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.2.Referenced Documents2.1 ASTM Standards:2D329 Specification for Acetone3.Significance and Use3.1 This
5、 test method is used by black pigment producers andusers for product acceptance.4.Apparatus4.1 Extraction Apparatus,consisting of a flask,siphon cup,and a condenser similar to the apparatus shown in either Fig.1or Fig.2.NOTE1A Sophlet apparatus may be used as an alternative.4.2 Extraction ThimblesTh
6、e thimble must be made ofgreaseless paper and be of correct size to fill the selectedapparatus.NOTE2The recommended thimble size for each of the apparatusshown in Fig.1 is listed below:Fig.1Fig.2Height70 mm62 mmInside diameter28 mm22 mmOutside diameter30 mm24 mm4.3 The thimbles are available in vari
7、ous heights and widthswith two thickness levels,single thickness or double thickness.Single-thickness thimbles are recommended for this extractionprocedure.5.Reagents and Material5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall
8、 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 use without lessening
9、 theaccuracy of the determination.5.2 SolventAcetone and benzene are the most commonlyused solvents(see Specification D329);however,other sol-vents may be used as agreed upon.5.3 Glass Wool.6.Procedure6.1 Weight approximately 10 g of pigment(moisture-free)into a weighed thimble and record the weight
10、 to 0.1 g.Forpigments with high apparent density(bone black,iron oxides,etc.)a 40-g sample is recommended.Plug the open end of thethimble with glass wool and place in the siphon cup.Add 200to 250 mL of the solvent to the previously dried flask.6.2 When using acetone as the extraction solvent,extract
11、continuously for 4 h,heating at a rate such that the timerequired to fill and empty the siphon cup will not exceed 8 min.With other solvents extract for 16 h.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct re
12、sponsibility ofSubcommittee D01.31 on Pigment Specifications.Current edition approved Dec.1,2014.Published December 2014.Originallyapproved in 1929.Last previous edition approved in 2008 as D305 84(2008).DOI:10.1520/D0305-84R14.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcon
13、tact 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 on the testing of reage
14、nts 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Con
15、shohocken,PA 19428-2959.United States1 NOTE3If particles of carbon have escaped from the cup into theextraction liquid,filter the liquid,wash the paper with solvent,and returnthe total filtrate to the extraction flask,prior to continuing with 6.3.6.3 Transfer quantitatively the extract solution to a
16、 400-mLbeaker that has been weighed to the nearest 0.1 g,andevaporate off the solvent on a steam bath or plate.Remove thebeaker from the bath or hot plate just before the last trace of thesolvent disappears.Dry the dish for 1 h at 105C(221F).Cooland weigh to the nearest 0.1 g.7.Calculation7.1 Calculate the percent extractable material,E,to thenearest 0.05%as follows:E 5R 2 B!/S 2 W!#3100(1)where:R=weight of extractable material and weighed dish,g,B=weight of weighed dish,g,S=weight of thimble an