ASTM_D_4358_-_05.pdf

Designation:D 4358 05Standard Test Method forLead and Chromium in Air Particulate Filter Samples ofLead Chromate Type Pigment Dusts by Atomic AbsorptionSpectroscopy1This standard is issued under the fixed designation D 4358;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 determines amounts of lead andchromium in residues obtained from air sampling of leadchromate and lead silico-chromate type pigment dusts.It is notapplicable to all pigment dusts or to paint overspray samples ofany kind.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,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:2D 1193 Specification for Reagent Water3.Summary of Test Method3.1 The filter containing the air particulate sample is dis-solved with nitric acid followed by treatment with 50%aqueous ammonium acetate solution.The solution is trans-ferred to a volumetric flask and lead and chromium determinedby atomic absorption.4.Significance and Use4.1 This test method covers only the analysis of the pigmentdusts on filters,the results being expressed as micrograms oflead and of chromium.Sampling procedures are not a part ofthis test method,nor are those calculations that are required toconvert the results to concentration of lead and chromium inthe sampled air,as required by the U.S.Occupational Safetyand Health Act(OSHA).5.Apparatus5.1 Atomic Absorption Spectrophotometer,consisting of anatomizer and burner;gas pressure regulating and meteringdevices for air,acetylene,and nitrous oxide;provision forhollow cathode source lamps with regulated constant currentsupply;a monochromator with associated optics;a photode-tector;an amplifier;and digital or analog readout system.5.2 Lead Hollow Cathode Lamp or electrodeless dischargesource lamp.5.3 Chromium Hollow Cathode Source Lamp.5.4 Volumetric Flasks,10-mL.6.Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the Committee on AnalyticalReagents of the American Chemical Society,where suchspecifications are available.3Other 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.6.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conformingto Type II of Specification D 1193.6.3 Ammonium Acetate Solution(50%W/V aqueous)Dissolve 250 g of ammonium acetate(NH4C2H3O2)in waterand dilute to 500 mL.6.4 Nitric Acid(sp gr 1.50)Concentrated nitric acid(HNO3).6.5 Nitric Acid,(1+3)Dilute 1 part concentrated nitricacid with 3 parts water.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved Jan.1,2005.Published February 2005.Originallyapproved in 1984.Last previous edition approved in 1999 as D 4358 84(1999).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.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.6.6 Lead,Standard Stock Solution(1000 g/mL)Dissolve0.1599 g of lead nitrate(Pb(NO3)2)in 50 mL of watercontaining 20 mL of concentrated HNO3and 10 mL of 50%ammonium acetate solution,and dilute to 100 mL with water.6.7 Chromium,Standard Stock Solution(1000 g/mL)Dissolve 0.3734 g of potassium chromate(K2CrO4)in 50 mLwater containing 5 mL of concentrated HNO3and dilute to 100mL with water.6.8 Filter BlankMillipore 0.8-m pore size,37-mm diam-eter,mixed esters of cellulose,Type AA white,plain,orequivalent.6.9 Hydrogen Peroxide30%(H2O2).7.Calibration and Standardization7.1 Good atomic absorption practice requires that the testsolutio