ASTM_D_4309_-_12.pdf

Designation:D430912Standard Practice forSample Digestion Using Closed Vessel Microwave HeatingTechnique for the Determination of Total Metals in Water1This standard is issued under the fixed designation D4309;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.Scope*1.1 This practice covers the general considerations forquantitative sample digestion for total metals in water usingclosed vessel microwave heating technique.This practice isapplicable to surface,saline,domestic,and industrial waste-water.1.2 Because of the differences among various makes andmodels of satisfactory instruments,no detailed operating in-structions can be provided.Instead,the analyst should followthe instructions provided by the manufacturer of the particularinstrument.1.3 This practice can be used with the following ASTMstandards,providing the user determines precision and biasbased on this digestion practice:Test Method D857,TestMethods D858,Test Methods D1068,Test Methods D1687,Test Methods D1688,Test Methods D1691,Test MethodsD1886,Test Method D1976,Practices D3370,Test MethodsD3557,Test Methods D3559,Practice D3919,Test MethodD4190,Practice D4453,Practice D4691,and Test MethodD5673.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 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.For specific hazardstatements,see Section 9.2.Referenced Documents2.1 ASTM Standards:2D857 Test Method for Aluminum in WaterD858 Test Methods for Manganese in WaterD1068 Test Methods for Iron in WaterD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD1687 Test Methods for Chromium in WaterD1688 Test Methods for Copper in WaterD1691 Test Methods for Zinc in WaterD1886 Test Methods for Nickel in WaterD1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission SpectroscopyD3370 Practices for Sampling Water from Closed ConduitsD3557 Test Methods for Cadmium in WaterD3559 Test Methods for Lead in WaterD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD3919 Practice for Measuring Trace Elements in Water byGraphite Furnace Atomic Absorption SpectrophotometryD4190 Test Method for Elements in Water by Direct-CurrentPlasma Atomic Emission SpectroscopyD4453 Practice for Handling of High Purity Water SamplesD4691 Practice for Measuring Elements in Water by FlameAtomic Absorption SpectrophotometryD5673 Test Method for Elements in Water by InductivelyCoupled PlasmaMass Spectrometry2.2 U.S.Code of Federal Regulations:3CFR 1.030.10 Code of Federal Regulations,Volume 212.3 Federal Communications Commission Standard:3Code of Federal Regulations,Volume 47,FCC Rule Part 181This practice is under the jurisdiction of ASTM Committee D19 on Water andis the direct responsibility of Subcommittee D19.05 on Inorganic Constituents inWater.Current edition approved March 1,2012.Published March 2012.Originallyapproved in 1991.Last previous edition approved in 2007 as D4309 02(2007).DOI:10.1520/D4309-12.2For 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.3Available from U.S.Government Printing Office Superintendent of Documents,732 N.Capitol St.,NW,Mail Stop:SDE,Washington,DC 20401,http:/www.access.gpo.gov.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 2.4 U.S.EPA Method:4U.S.EPA Method:Methods for Chemical Analysis of Waterand WasteMarch 1979,“Total Metals Digestion Proce-dure”4.1.3,page Metals 6U.S.EPA Method:SW 846 Method 3015 Microwave As-sisted Acid Digestion of Aqueous Samples and Extracts3.Terminology3.1 DefinitionsFor definitions of terms used in thispractice,refer to Terminology D1129.4.Summary of Practice4.1 A representative aliquot of a homogeneous sample isdigested with acid in a closed microwave transparent vessel,using microwave heating.The digestate or a filtered digestateis then analyzed by direct aspiration or injection by flameatomic absorption spectrophotometry(FAAS),inductivelycoupled plasma emission techniques(ICP),direct currentplasma emission techniques(DCP),graphite furnace atomicabsorption spectrophotometry(GFAAS),inductively coupledplasma-mass spectrometry(ICP-MS),or a combination ofmethods.5.Significance and Use5.1 The analysis of many