ASTM_D_4744_-_89_1995e1.pdf

Designation:D 4744 89(Reapproved 1995)e1Standard Test Method forOrganic Halides in Water by CarbonAdsorptionMicrocoulometric Detection1This standard is issued under the fixed designation D 4744;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.e1NOTESection 15 was added editorially in June 1995.1.Scope1.1 This test method covers the determination of the organichalides in water in concentrations from 5 to 1000 g/L.Higherhalide concentrations may be determined by making an appro-priate dilution.1.2 This test method is applicable only for those organichalides that can be adsorbed by granular activated carbon(GAC).2,3,41.3 This test method is applicable to samples whose inor-ganic halide concentration does not exceed the organic halideconcentration by more than 20 000 times.Chloride ion may bedetermined by Test Methods D 512.See Section 6.1.4 This test method was used successfully with severalwaters(see 14.3).It is the users responsibility to ensure thevalidity of this test method for waters of untested matrices.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.2.Referenced Documents2.1 ASTM Standards:D 512 Test Methods for Chloride Ion in Water5D 1129 Terminology Relating to Water5D 1193 Specification for Reagent Water5D 2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D-19 on Water53.Terminology3.1 DefinitionsFor definitions of terms used in this testmethod,refer to Terminology D 1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 organic halidesall organic species containing chlo-rine,bromine,and iodine that are adsorbed by granularactivated carbon and produce titratable species under theconditions of the test method.See Section 6.3.2.2 Since the description of organic halides is method-dependent,the following descriptions are provided to simplifycommunications.3.2.3 total organic halides(TOX)when a sample is rununpurged and unfiltered,the result is called total organichalides(TOX).3.2.4 nonpurgeable organic halides(NPOX)when asample is purged before running,the result is called nonpurge-able organic halides(NPOX).3.2.5 purgeable organic halides(POX)the difference be-tween the TOX and the NPOX is the purgeable organic halides(POX).The POX fraction may also be determined directly bya variation of this test method.3.2.6 dissolved organic halides(DOX)when a samplecontaining some solid material is filtered or centrifuged and theliquid portion is analyzed,the result is called dissolved organichalides(DOX).3.2.7 suspended organic halides(SOX or SX)when thesolid material is resuspended in TOX-free water and analyzed,the result is called suspended organic halides(SOX).Since thistest method is not designed to specifically remove inorganichalides from suspended matter,this measurement may moreproperly be called suspended halides(SX).It should be notedthat DOX and SX results are highly dependent upon the type offiltration or centrifugation process used.4.Summary of Test Method4.1 This test method consists of three steps.These are thefollowing:4.1.1 Adsorption of organics from water onto granularactivated carbon(GAC)packed in microcolumns,4.1.2 Desorption of inorganic halides by washing the GACwith nitrate solution,and4.1.3 Combustion of sorbed organics along with the GAC,1This test method is under the jurisdiction of ASTM Committee D-19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved Nov.24,1989.Published March 1990.Originallypublished as D 4744 87.Last previous edition D 4744 87.2Belford,G.,“Absorption on Carbon:Theoretical Considerations,Environ-mental Science and Technology,August 1980,p.910.3Dobbs,R.,and Cohen,J.,“Carbon Adsorption Isotherms for Toxic Organics,”EPA600/8-80-023,April 1980,National Technical Information Center,Springfield,VA 22161.4Fochtman,E.,and Dobbs,R.,Adsorption of Carcinogenic Compounds byActivated Carbon,Activated Carbon Adsorption of Organics from the AqueousPhase,Vol 1,Ann Arbor Science,Ann Arbor,MI,p.157.5Annual Book of ASTM Standards,Vol 11.01.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTMfollowed by microcoulometric titration against silver ion ofhalides thus produced.4.2 The procedure may be further detailed as follows:4.2.1 First,sodium sulfite is added to a water sample toreduce any residual chlorine to chloride.The sample is thenacidified to pH 2 with nitric acid to i