ASTM_D_6156_-_97.pdf

Designation:D 6156 97An American National StandardStandard Practice forUse of Reversed-Phase High Performance LiquidChromatographic Systems1This standard is issued under the fixed designation D 6156;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 practice covers requirements for defining,testing,and verifying the performance of high performance liquidchromatographic(HPLC)systems when used for trace analysisof pesticides and toxic substances in carrying out pollutioncontrol programs and in assessing the quality of food productsas mandated by national laws and regulations.As a practicalmatter,this practice is intended to cover requirements ofreversed-phase(adsorption)HPLC systems.Microbore columnand ion-exchange column HPLC systems are not covered here.It is not intended to exclude any other equivalent means ofanalysis.An HPLC system can successfully be applied in theanalysis of a variety of sample types including ground andsurface water,municipal and industrial effluents,workplace air,soils and sediments,plant and animal tissue,and food products(1,2,3).2Collection and extraction techniques,appropriate tothe sample type,are required prior to analysis.Samplingtechniques and measurement methods are not covered in thisrecommendation;however,some relevant measurement meth-ods may be found in references listed in Appendix X1.NOTE1High performance liquid chromatography is synonymouswith high pressure liquid chromatography.1.2 Metrological and technical requirements are providedfor the major components of an HPLC system including thepump(s),injector(s),column(s),detector(s),and temperaturecontrol and data handling systems.The conditions of operationof a single integrated instrument,or one combined fromseparate components,are intended to cover the application fortrace analysis.1.3 Basically four types of packed columns for liquidchromatography exist:partition,adsorption,ion exchange,andgel permeation.Other terms are used to refer to each type.Formany separations,however,the actual separation may not beclearly defined and may involve a combination of retentionmechanisms.Furthermore,the polarity of the stationary phasecan be greater or less than the mobile phase.The separationmethod is called normal-phase HPLC when the stationaryphase is more polar than the mobile phase,and the separationmethod is called reversed-phase HPLC when the reversecondition exists.The reversed-phase HPLC system,using anadsorption column,has become the more frequently usedtechnique for separation and analysis of organic compounds.Itcan separate a broad spectrum of nonionic,ionizable,and ioniccompounds,and its columns are usually stable and separationsmay be performed with good repeatability since the stationaryphases are chemically bonded.1.4 The detector type selected for use with an HPLC systemdepends generally on the concentration as well as the chemicaland physical properties of the sample matrix and the analyte tobe measured.The following detectors are covered in thispractice.UV/Visible spectrophotometric,fluorescence,electro-chemical,and refractive index.NOTE2The mass spectrometer is a highly specific and sensitivedetector appropriate for most applications.It is normally coupled to theHPLC system through an appropriate interface.The use of a massspectrometer as a detector is not covered in this practice because of itsspecialized nature.1.5 The following are examples of classes of analytes thatmay be measured by an HPLC system:carbamates,pyrethri-ods,organophosphates,polycyclic aromatic hydrocarbons,phenolics,isocyanates,aflatoxins,chlorophenoxy-acid herbi-cides,triazine herbicides,and amines.An advantage of HPLCover gas chromatography is that it may be used for the directmeasurement of thermally labile compounds,compounds oflow volatility,and strongly polar compounds without conver-sion to derivatives.1.6 Optimizing the performance of each major componentof the measuring system may achieve performance better thatthe criteria prescribed for these applications.Success in thisrespect depends on the knowledge,skill,and experience of theanalyst.1.7 The values stated in SI units are to be regarded as thestandard.1This practice is under the jurisdiction of ASTM Committee D-19 on Water andis the direct responsibility of Subcommittee D19.06 on Methods for Analysis forOrganic Substances in Water.Current edition approved July 10,1997.Published October 1997.2The boldface numbers given in parentheses refer to a list of references at theend of the text.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.1.8 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the use