ASTM_D_3223_-_12.pdf

Designation:D322312Standard Test Method forTotal Mercury in Water1This standard is issued under the fixed designation D3223;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.Scope*1.1 This test method2covers the determination of totalmercury in water in the range from 0.5 to 10.0 g Hg/L(1).3The test method is applicable to fresh waters,saline waters,andsome industrial and sewage effluents.It is the users responsi-bility to ensure the validity of this test method for waters ofuntested matrices.1.1.1 The analyst should recognize that the precision andbias of this standard may be affected by the other constituentsin all waters,as tap,industrial,river,and wastewaters.The coldvapor atomic absorption measurement portion of this method isapplicable to the analysis of materials other than water(sediments,biological materials,tissues,etc.)if,and only if,aninitial procedure for digesting and oxidizing the sample iscarried out,ensuring that the mercury in the sample isconverted to the mercuric ion,and is dissolved in aqueousmedia(2,3).1.2 Both organic and inorganic mercury compounds may beanalyzed by this procedure if they are first converted tomercuric ions.Using potassium persulfate and potassiumpermanganate as oxidants,and a digestion temperature of95C,approximately 100%recovery of organomercury com-pounds can be obtained(2,4).1.3 The range of the test method may be changed byinstrument or recorder expansion or both,and by using a largervolume of sample.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 Amethod for the disposal of mercury-containing wastesis also presented(Appendix X1)(5).1.6 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 and.2.Referenced Documents2.1 ASTM Standards:4D512 Test Methods for Chloride Ion In WaterD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD1245 Practice for Examination of Water-Formed Depositsby Chemical MicroscopyD1252 Test Methods for Chemical Oxygen Demand(Di-chromate Oxygen Demand)of WaterD1426 Test Methods for Ammonia Nitrogen In WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD4691 Practice for Measuring Elements in Water by FlameAtomic Absorption SpectrophotometryD4841 Practice for Estimation of Holding Time for WaterSamples Containing Organic and Inorganic ConstituentsD5810 Guide for Spiking into Aqueous SamplesD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water Analysis3.Terminology3.1 Definitions:For definitions of terms used in this testmethod,refer to Terminology D1129.4.Summary of Test Method4.1 The test method consists of a wet chemical oxidationwhich converts all mercury to the mercuric ion;reduction ofmercuric ions to metallic mercury,followed by a cold vaporatomic absorption analysis(1,2).Ageneral guide for flame andvapor generation atomic absorption applications is given inPractice D4691.1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.05 on Inorganic Constituentsin Water.Current edition approved Sept.1,2012.Published September 2012.Originallyapproved in 1979.Last previous edition approved in 2002 as D3223 02(2007)1.DOI:10.1520/D3223-12.2Adapted from research investigations by the U.S.Environmental ProtectionAgencys Analytical Quality Control Laboratory,Cincinnati,OH,and Region IVSurveillance and Analysis Division,Chemical Services Branch,Athens,GA.3The boldface numbers in parentheses refer to the references at the end of thistest method.4For 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.*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 4.2 Cold vapor atomic absorption analysis is a physicalmethod based on the absorption of ultraviolet radiation at awavelength of 253.7 nm by mercury vapor.The mercury isreduced to the elemental state and aerated from solution ineither a closed recirculating system or an open one-passsystem.The mercury vapor passes