ASTM_D_49_-_83_2014.pdf

Designation:D4983(Reapproved 2014)Standard Test Methods ofChemical Analysis of Red Lead1This standard is issued under the fixed designation D49;the number immediately following the designation indicates the year of originaladoption or,in the case of revision,the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscriptepsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 These test methods cover procedures for the chemicalanalysis of red lead having the approximate formula Pb3O4(probably PbO22PbO).1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 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 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:2D50 Test Methods for ChemicalAnalysis of Yellow,Orange,Red,and Brown Pigments Containing Iron and Manga-neseD215 Practice for the Chemical Analysis of White LinseedOil Paints(Withdrawn 2005)3D280 Test Methods for Hygroscopic Moisture(and OtherMatter Volatile Under the Test Conditions)in PigmentsD1193 Specification for Reagent WaterD1208 Test Methods for Common Properties of CertainPigmentsD1301 Test Methods for Chemical Analysis of White LeadPigmentsD1959 Test Method for Iodine Value of Drying Oils andFatty Acids(Withdrawn 2006)33.Treatment of Sample3.1 If the pigment is lumpy or not finely ground,grind it toa fine powder and mix thoroughly.Large samples may bethoroughly mixed and a representative portion taken andpowdered if lumpy or not finely ground.The sample in allcases shall be thoroughly mixed before taking portions foranalysis.All samples shall be preserved in stoppered bottles orcontainers.4.Purity of Reagents4.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated,it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society where suchspecifications are available.4Other grades may be used pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.4.2 Unless otherwise indicated,references to water shall beunderstood to mean reagent water conforming to Type II ofSpecification D1193.5.Moisture5.1 Determine moisture content with a 2-g specimen inaccordance with Method A of Test Methods D280.Thespecimen is dried for 2 h at 105C.The loss in weight isconsidered as moisture.6.Organic Color6.1 Boil 2 g of the sample with 25 mLof 95%ethyl alcohol,let settle,decant the supernatant liquid;boil the residue with 25mL of distilled water and decant as before;boil the residuewith 25 mL of diluted NH4OH(1+4)and again decant.Boilanother 2-g portion of the sample with 25 mL of chloroform,let settle,and decant the supernatant liquid.If any one of theabove solutions is colored,organic coloring matter is indicated.If the solutions remain colorless,organic colors are probablyabsent.NOTE1If it is desired to test for organic colors resistant to the abovereagents,the test procedures described in the following books may be1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings,Materials,and Applications and are the directresponsibility of Subcommittee D01.31 on Pigment Specifications.Current edition approved Dec.1,2014.Published December 2014.Originallyapproved in 1917.Last previous edition approved in 2008 as D49 83(20081).DOI:10.1520/D0049-83R0814.2For referenced ASTM standards,visit the ASTM website,www.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.3The last approved version of this historical standard is referenced onwww.astm.org.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,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 Conshohocken,PA 19428-2959.United States1 used,taking into account the nature of the pigment involved(1,2,3).57.Total Lead and Insoluble Matter7.1 Treat 1 g of the sample with 15 mL of HNO3(1+1)andsufficient H2O2to dissolve all PbO2on warming.If anyinsoluble matter is present,add 25 mL of water,boil,filter,andwash with hot water.The insoluble matter contains free SiO2and should be examined for BaSO4and silicates,if appre-ciable.7.2 To the original solution or filtrate from the insolublematter add 20 mL of H2