ASTM_D_1394_-_76_2014.pdf

Designation:D139476(Reapproved 2014)Standard Test Methods forChemical Analysis of White Titanium Pigments1This standard is issued under the fixed designation D1394;the number immediately following the designation 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()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 These test methods cover procedures for the chemicalanalysis of white titanium dioxide pigments.1.2 The analytical procedures appear in the following order:SectionsPreparation of Sample4Qualitative Analysis5 and 6Moisture7Total Titanium:Jones Reductor Method8 12Aluminum Reduction Method13 17Aluminum Oxide18 22Silica23 291.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 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.A specific hazardstatement is given in Section 19.2.Referenced Documents2.1 ASTM Standards:2D280 Test Methods for Hygroscopic Moisture(and OtherMatter Volatile Under the Test Conditions)in PigmentsD1193 Specification for Reagent WaterE50 Practices for Apparatus,Reagents,and Safety Consid-erations for Chemical Analysis of Metals,Ores,andRelated Materials3.Reagents3.1 Purity of ReagentReagent 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.3Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.3.2 Unless otherwise indicated,references to water shall beunderstood to mean reagent water conforming to Type IV ofSpecification D1193.4.Preparation of Sample4.1 The sample shall,in all cases,be thoroughly mixed andcomminuted before taking portions for analysis.QUALITATIVE ANALYSIS5.Reagents5.1 Ammonium Hydroxide(sp gr 0.90)Concentrated am-monium hydroxide(NH4OH).5.2 Ammonium Sulfate(NH4)2SO4).5.3 Hydrochloric Acid(sp gr 1.19)Concentrated hydro-chloric acid(HCl).5.4 Hydrogen Peroxide(30%)Concentrated hydrogenperoxide(H2O2).5.5 Hydrogen Sulfide(H2S).5.6 Sulfuric Acid(sp gr 1.84)Concentrated sulfuric acid(H2SO4).5.7 Sulfuric Acid(1+19)Carefully mix 1 volume ofH2SO4(sp gr 1.84)with 19 volumes of water.5.8 Tartaric Acid.5.9 Tin or Zinc Metal.1These 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 1956.Last previous edition approved in 2009 as D1394 76(2009).DOI:10.1520/D1394-76R14.2For 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.3Reagent 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 6.Procedure6.1 Place about 0.5 g of the sample in a 250-mL glassbeaker,4and add 20 mL of H2SO4(sp gr 1.84)and 7 to 8 g of(NH4)2SO4.Mix well and boil for a few minutes.The sampleshould go completely into solution;a residue denotes thepresence of silicon dioxide(SiO2)or siliceous matter.Cool thesolution,dilute with 100 mL of water,heat to boiling,let settle,filter,wash with hot H2SO4(1+19)until free of titanium,andtest the residue for lead,etc.6.2 Test the filtrate for calcium,zinc,iron,chromium,etc.,by the regular methods of qualitative analysis.5For the irondetermination add to a portion of the filtrate 5 g of tartaric acid,render slightly ammoniacal,pass in H2S in excess,and digeston a steam bath.No precipitate after 30 min indicates theabsence of iron,nickel,cobalt,lead,copper,etc.A blackprecipitate readily soluble in dilute HCl denotes iron.Fortitanium,test a small portion of the original filtrate with H2O2(a clear yellow-orange color should result)and another portionwith metallic tin or zinc(a pale blue to violet coloration shouldresult).Negative