ASTM_D_6800_-_12.pdf

Designation:D680012Standard Practice forPreparation of Water Samples Using Reductive PrecipitationPreconcentration Technique for ICP-MS Analysis of TraceMetals1This standard is issued under the fixed designation D6800;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 Toxic elements may be present in ambient waters andmay enter the food chain via uptake by plants and animals;theactual concentrations of toxic metals are usually sub-ng/mL.The U.S.EPA has published its Water Quality Standards in theU.S.Federal Register 40 CFR 131.36,Minimum requirementsfor water quality standards submission,Ch.I(7-1-00 Edition),see Annex,Table A1.1.The U.S.EPA has also developedMethod 1640 to meet these requirements,see Annex,TableA1.2.1.2 Inductively Coupled Plasma Mass Spectroscopy(ICP-MS)is a technique with sufficient sensitivity to routinelymeasure toxic elements in ambient waters,both fresh andsaline(Test Method D5673).However saline and hard watermatrices pose analytical challenges for direct multielementanalysis by ICP-MS at the required sub-ng/mL levels.1.3 This standard practice describes a method used toprepare water samples for subsequent multielement analysisusing ICP-MS.The practice is applicable to seawater and freshwater matrices,which may be filtered or digested.Samplesprepared by this method have been analyzed by ICP-MS for theelements listed in Annex,Table A1.3).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.2.Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD5673 Test Method for Elements in Water by InductivelyCoupled PlasmaMass SpectrometryD5810 Guide for Spiking into Aqueous SamplesD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water Analysis2.2 Other Documents:U.S.Federal Register 40 CFR 131.36,Minimum Require-ments for Water Quality Standards Submission,Ch.I(7-1-00 Edition)3U.S.EPA Method 1640,Determination of Trace Elements inWater by Preconcentration and Inductively CoupledPlasma-Mass Spectrometry(1997)4U.S.EPA Method 1669,Sampling Ambient Water for TraceMetals at EPA Water Quality Criteria Levels43.Terminology3.1 DefinitionsFor definitions of terms used in this testmethod refer to Terminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 intermediate stock-standard solution,na diluted so-lution prepared from one or more of the stock-standardsolutions.3.2.2 laboratory control sample(LCS),nan aliquot ofsolution with known concentrations of method analytes.1This 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 2002.Last previous edition approved in 2007 as D6800 02(2007)e01.DOI:10.1520/D6800-12.2For 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 DODSSP,Bldg.4,Section D,700 Robbins Ave.,Philadelphia,PA 191115098.4Available from United States Environmental Protection Agency(EPA),ArielRios Bldg.,1200 Pennsylvania Ave.,NW,Washington,DC 20460,http:/www.epa.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 3.2.2.1 DiscussionThe LCS should be obtained from areputable source or prepared at the laboratory from a separatesource from the calibration standards.The LCS is analyzedusing the same sample preparation,analytical method andQA/QC procedure used for test samples.Its purpose is todetermine whether method performance is within acceptedcontrol limits.3.2.3 laboratory duplicate(LD),na second sample aliquotthat is analyzed using the same sample preparation,analyticalmethod and QA/QC procedure used for test samples.3.2.3.1 DiscussionThe purpose of the LD is to determinewhether method performance is within accepted control limits.3.2.4 matrix spike(MS),na second sample aliquot towhich known concentrations of target analyte(s)are added inthe laboratory and which are analyzed using the same samplepreparation and analytical method used for test samples.3.2.4.1 DiscussionThe purpose of the MS is t