ASTM_D_7511_-_12.pdf

Designation:D751112Standard Test Method forTotal Cyanide by Segmented Flow Injection Analysis,In-LineUltraviolet Digestion and Amperometric Detection1This standard is issued under the fixed designation D7511;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 method is used for determining total cyanide indrinking and surface waters,as well as domestic and industrialwastes.Cyanide ion(CN-),hydrogen cyanide in water(HCN(aq),and the cyano-complexes of zinc,copper,cadmium,mercury,nickel,silver,and iron may be determinedby this method.Cyanide ions from Au(I),Co(III),Pd(II),andRu(II)complexes are only partially determined.1.2 The method detection limit(MDL)is 1.0 g/L cyanideand the minimum level(ML)is 3 g/L.The applicable range ofthe method is 3 to 500 g/L cyanide using a 200-L sampleloop.Extend the range to analyze higher concentrations bysample dilution or changing the sample loop volume.1.3 This method can be used by analysts experienced withequipment using segmented flow analysis(SFA)and flowinjection analysis(FIA)or working under the close supervisionof such qualified persons.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.Specific hazardstatements are given in Note 2 and Section 9.2.Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2036 Test Methods for Cyanides in WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD4210 Practice for Intralaboratory Quality Control Proce-dures and a Discussion on Reporting Low-Level Data(Withdrawn 2002)3D5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisD6696 Guide for Understanding Cyanide SpeciesD7365 Practice for Sampling,Preservation and MitigatingInterferences in Water Samples for Analysis of Cyanide3.Terminology3.1 Definitions:3.1.1 For definitions of terms used in this test method,referto Terminology D1129 and Guide D6696.3.1.2 total cyaniderefers to all cyanide-containing com-pounds in a sample,including free cyanide,WAD cyanidecompounds,and strong metal cyanide complexes.4.Summary of Test Method4.1 Prior to analysis,treat the sample to remove potentialinterferences(Sections 4 and 8).Ultraviolet(UV)digestionreleases cyanide from cyanide complexes.Acid addition con-verts cyanide ion to hydrogen cyanide gas(HCN),whichpasses under a gas diffusion membrane.The hydrogen cyanidegas diffuses through the membrane into an alkaline receivingsolution,where it converts back to cyanide ion.A silverworking electrode,silver/silver chloride reference electrode,and platinum/stainless steel counter electrode at an appliedpotential of zero volt amperometrically monitor the cyanideion.The current generated is proportional to the cyanideconcentration present in the original sample.4.2 Calibrations and data are processed with the instru-ments data acquisition software.1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved Jan.1,2012.Published January 2012.Last previousedition published 2009 as D751109E01.DOI:10.1520/D7511-12.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.Significance and Use5.1 Cyanide and hydrogen cyanide are highly toxic.Regu-lations have been established to require the monitoring ofcyanide in industrial and domestic wastewaters and surfacewaters.45.2 This test method is applicable for natural water,salinewaters,and wastewater effluent.5.3 The method may be used for process control in waste-water treatment facilities.5.4 The spot test outlined in Test Methods D2036,AnnexA1 can be used to detect cyanide and thiocyanate in water orwastewater,and to approximate its concentration.6.Interferences6.1 Method interferences can be caused by contami