ASTM_D_5475_-_93_2002.pdf

Designation:D 5475 93(Reapproved 2002)An American National StandardStandard Test Method forNitrogen-and Phosphorus-Containing Pesticides in Waterby Gas Chromatography with a Nitrogen-PhosphorusDetector1This standard is issued under the fixed designation D 5475;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.1.Scope1.1 This is a gas chromatographic(GC)test method appli-cable to the determination of certain nitrogen-and phosphorus-containing pesticides in ground water and finished drinkingwater.2The analytes listed in Table 1 have been validated usingthis test method.1.2 This test method has been validated on reagent waterand finished drinking water by 10 volunteer laboratories.Summary statistics were calculated for mean recovery,overallmethod precision and bias and single analyst precision using acomputer program,Interlaboratory Method Validation Study(IMVS).21.3 Collaborative study showed the test method to beacceptable for all analytes tested except merphos,whichdecomposed in the GC injection port.1.4 This test method is restricted to use by or under thesupervision of analysts experienced in the use of GC and in theinterpretation of gas chromatograms.Each analyst must dem-onstrate the ability to generate acceptable results with this testmethod using the procedure described in 12.3.1.5 Analytes that are not separated chromatographically,that is,analytes which have very similar retention times,cannotbe individually identified and measured in the same calibrationmixture or water sample unless an alternative technique foridentification and quantitation exist(13.5).1.6 When this test method is used to analyze unfamiliarsamples for any or all of the analytes above,analyte identifi-cations should be confirmed by at least one additional qualita-tive technique.1.7 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 1129 Terminology Relating to Water3D 1192 Specification for Equipment for Sampling Waterand Steam in Closed Conduits3D 1193 Specification of Reagent Water3D 2777 Practice for Determination of Precision and Bias ofApplicable Methods of Committee D19 on Water3D 3370 Practices for Sampling Water from Closed Con-duits3D 3694 Practices for Preparation of Sample Containers andfor Preservation of Organic Constituents42.2U.S.EPA Method:EPA Method 507,Revision 2.0 Determination of Nitrogen-and Phosphorus-Containing Pesticides in Water by GasChromatography with a Nitrogen-Phosphorus Detector53.Terminology3.1 DefinitionsFor definitions of water terms used in thispractice,refer to Terminology D 1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 internal standarda pure analyte(s)added to a solu-tion in known amount(s)and used to measure the relativeresponses of other test method analytes and surrogates that arecomponents of the same solution.3.2.1.1 DiscussionThe internal standard must be an ana-lyte that is not a sample component.3.2.2 surrogate analytea pure analyte(s),which is ex-tremely unlikely to be found in any sample,and which is addedto a sample aliquot in known amount(s)before extraction andis measured with the same procedures used to measure othersample components.3.2.2.1 DiscussionThe purpose of a surrogate analyte is tomonitor test method performance with each sample.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 Dec.15,1993.Published March 1994.Originallypublished as D 5475 93.Last previous edition D 5475 93(1997).2Edgell,K.W.,Jenkins,E.L.,Lopez-Avila,V.,and Longbottom,J.,“CapillaryColumn Gas Chromatography with Nitrogen-Phosphorus Detection for Determina-tion of Nitrogen-and Phosphorus-Containing Pesticides in Finished DrinkingWaters:Collaborative Study,”Journal of Association of Official Analytical Chem-ists,Vol 74,1991,pp.295309.3Annual Book of ASTM Standards,Vol 11.01.4Annual Book of ASTM Standards,Vol 11.02.5Available as part of publication PB91231480 from National TechnicalInformation Service,5285 Port Royal Road,Springfield,VA 22161.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.3.2.3 laboratory duplicates(LD1 and LD2)two samplealiquots taken in the analytical laboratory and analyzed sepa-rately with identical procedures.3.2.3.1 DiscussionAnalyses of LD1 and LD2 give ameasure of the precision with laboratory procedures,but notwith sample collection,preservatio