ASTM_D_3717_-_85a_2015.pdf

Designation:D371785a(Reapproved 2015)Standard Test Method forLow Concentrations of Antimony in Paint by AtomicAbsorption Spectroscopy1This standard is issued under the fixed designation D3717;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.1.Scope1.1 This test method covers the determination of the contentof antimony in the range between 50 and 200 ppm(mg/kg)present in the solids of liquid coatings or in dried filmsobtained from previously coated substrates.There is no reasonto believe that higher levels could not be determined by thistest method,provided that appropriate dilutions and adjust-ments in specimen size and reagent quantities are made.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.Specific hazardstatements are given in Section 7.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD2832 Guide for Determining Volatile and Nonvolatile Con-tent of Paint and Related Coatings3.Summary of Test Method3.1 The sample of liquid coating or dried film is preparedfor analysis by dry ashing at 500C,followed by refluxing withhydrochloric acid and stannous chloride.The antimony contentof the acid extract is determined by atomic absorption spec-troscopy.4.Significance and Use4.1 The permissible level of heavy metals in certain coat-ings is specified by governmental regulatory agencies.This testmethod provides a fully documented procedure for determininglow concentrations of antimony present in both water-andsolvent-reducible coatings to determine compliance.5.Apparatus5.1 Atomic Absorption Spectrophotometer,consisting of anatomizer and either a single-or three-slot burner;gas pressureregulating and metering devices for air and acetylene;anantimony source lamp with a regulated constant current supply;a monochromator and associated optics;a photosensitivedetector connected to an electronic amplifier;and a readoutdevice.5.2 Muffle Furnace,maintained at 500 6 10C.5.3 Oven,maintained at 105 6 2C.5.4 Hot-Plate,with variable surface temperature controlover the range from 70 to 200C.5.5 Reflux Condenser,water-cooled,and fitted with astandard-taper joint.5.6 Erlenmeyer Flask,125-mL,with standard-taper joint tofit condenser.5.7 Volumetric Flasks,100 and 1000-mL.5.8 Dropping Bottles,8 or 15-mL(14or12-oz)capacity.5.9 Glass or Disposable Syringes,10-mL capacity.5.10 Pipets,1,5,10,and 15-mL capacity.5.11 Filter Paper,ashless,medium or slow filtering.5.12 Paint Shaker.5.13 Paint Draw-Down Bar.6.Reagents6.1 Purity of ReagentsReagent 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,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 June 1,2015.Published June 2015.Originallyapproved in 1978.Last previous edition approved in 2010 as D3717 85a(2010).DOI:10.1520/D3717-85AR15.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 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.6.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent grade waterconforming to Type II of Specification D1193.6.3 Antimony Standard Stock Solution(0.1 mg/mL)Dissolve 0.1000 g of antimony metal in 40 mL of sulfuric acid(H2SO4,sp gr 1.84)by heating.Cool,carefully transferquantitatively to a 1-L volumetric flask already approximatelyhalf full with water,allow to cool to room temperature,anddilute to 1 L.6.4 Hydrochloric Acid(sp gr 1.19)Concentrated hydro-chloric acid(HCl).6.5 Stannous Chloride Solution(400 g/L in HCl)Dissolve40 g of tin(II)chloride(SnCl2)in 50 mL of HCl(sp gr 1.19).Transfer to a 100-mL volumetric flask and fill to the mark withconcentrated HCl.7.Hazards7.1 Use care in handling conc