ASTM_D_2348_-_02.pdf

Designation:D 2348 91(Reapproved 1996)1This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version.Becauseit may not be technically possible to adequately depict all changes accurately,ASTM recommends that users consult prior editions as appropriate.In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.Designation:D 2348 02Standard Test Method forArsenic in Paint1This standard is issued under the fixed designation D 2348;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the determination of less than 0.5%arsenic in whole paint.1.2 This standard does not purport to address all of the safety concerns,if any,associated with its use.It is the responsibilityof whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water23.Summary of Test Method3.1 The specimen of liquid paint is prepared for analysis by acid-digestion.The arsenic content of a distillate from theacid-digested sample is determined by titration with KBrO3solution.4.Significance and Use4.1 The permissible level of toxic elements in certain coatings is specified by governmental regulatory agencies.This testmethod provides a documented procedure for determining low concentrations of arsenic present in whole paint to determinecompliance.5.Apparatus5.1 Kjeldahl Flask,800-mL,with standard-taper 24/40 joint.5.2 Condenser Delivery Tube,with standard-taper 24/40 joint.5.3 Mechanical Shaker.5.4 Gas Burner,suitable for heating Kjeldahl flask.5.5 Glass or Disposable Syringes,2 mL capacity.5.6 Erlenmeyer Flasks,250 and 500 mL capacity.5.7 Pipets,10 mL capacity.6.Reagents6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests.Unless otherwise indicated,it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society,wheresuch specifications are available.3Other grades may be used,provided it is ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination.6.2 Purity of WaterUnless otherwise indicated,references to water shall be understood to mean reagent grade waterconforming to Type II of Specification D 1193.6.3 Arsenous Oxide,Standard SolutionDissolve 0.3241 g of arsenous oxide(As2O3)in 25 mL of sodium hydroxide(NaOH)solution(100 g/L).Make slightly acid with sulfuric acid(H2SO4,1+8),and dilute to 1.0 L with water.1This test method is under the jurisdiction of ASTM Committee D-1 D01 on Paint and Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Material.Current edition approved Oct.15,1991.Jan.10,2002.Published December 1991.March 2002.Originally published as D 2348 65 T.Last previous editionD 2348 8591(1996).2Annual Book of ASTM Standards,Vol 11.01.3Reagent Chemicals,American Chemical Society Specifications,American Chemical Society,Washington,DC.For suggestions on the testing of reagents not listed bythe American Chemical Society,see Analar Standards for Laboratory Chemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeia and NationalFormulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.D 2348 91(1996)26.4 Hydrazine Sulfate-Potassium Bromide SolutionDissolve 20 g of hydrazine sulfate(N2H4H2SO4)and 23 g of potassiumbromide(KBr)in 200 mL of concentrated hydrochloric acid(HCl,sp gr 1.19)(PrecautionWarningsee 7.1)and dilute to 1 L.6.5 Methyl Orange Indicator SolutionDissolve 0.1 g in 100 mL water.6.6 Nitric Acid(sp gr 1.42)Concentrated nitric acid(HNO3)(Precaution Warningsee 7.1).6.7 Potassium Bromate,Standard SolutionDissolve 0.18 g of potassium bromate(KBrO3)in water and dilute to 1 L withwater.Standardize as follows:Transfer 10.0 mL of standard arsenous oxide solution by pipet to a 250-mL flask.Add 100 mL ofwater and 25 mL of HCl(sp gr 1.19).Heat to 90C and titrate with KBrO3as described in 8.5.Calculate the standardization factor,F,as follows:F 50.0032410 3 0.7574!/V(1)where:0.0032410=As2O3in 10.0 mL of solution,g,0.7574=factor converting As2O3to As,andV=KBrO3required for the titration,mL.6.8 Sodium Chloride(NaCl).6.9 Sulfuric Acid(sp gr 1.84)Concentrated sulfuric acid(H2SO4)(PrecautionWarningsee 7.1).7.Hazards7.1 Handling concentrated acids can be hazardous.Refer